CN209619244U - Crude maleic anhydride continuous rectification apparatus - Google Patents
Crude maleic anhydride continuous rectification apparatus Download PDFInfo
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- CN209619244U CN209619244U CN201920340565.2U CN201920340565U CN209619244U CN 209619244 U CN209619244 U CN 209619244U CN 201920340565 U CN201920340565 U CN 201920340565U CN 209619244 U CN209619244 U CN 209619244U
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Abstract
The utility model relates to a kind of crude maleic anhydride continuous rectification apparatus after n butane oxidation-organic solvent absorbs parsing, belong to cis-butenedioic anhydride rectifying separation field.The crude maleic anhydride continuous rectification apparatus, distributor one end is connected with crude maleic anhydride line, the other end is connect by pipeline with cut light tower, is successively connect with cut light tower overhead condenser, cut light tower return tank and vacuum system at the top of cut light tower by pipeline；It successively adopts line with cut light tower reflux pump, preheater, mixer, hydrogenator, knockout drum, propionic acid tank, propionic acid pump and propionic acid by pipeline outside and connect in cut light tower return tank bottom end；Cut light tower bottom end is successively connected with cut light tower tower reactor pump, treating column, refined tower top condenser, treating column return tank, tail gas washing tower and vacuum system by pipeline；The device design science, it is structurally reasonable.
Description
Technical field
The crude maleic anhydride continuous rectification dress that the utility model relates to a kind of after n butane oxidation-organic solvent absorbs parsing
It sets, belongs to cis-butenedioic anhydride rectifying separation field.
Background technique
Cis-butenedioic anhydride also known as maleic anhydride, apple anhydride dehydration are the third-largest acid for being only second to phthalic anhydride and aceticanhydride in the world at present
Acid anhydride.The production method of China Maleic Anhydrite can be divided into benzene oxidatoin method, n butane oxidation method by raw material route.N butane oxidation method has ring
The advantages that border pollution small, carbon atom utilization rate is high, raw material sources are extensive and cheap, in recent years just gradually substituted benzene oxidizing process
Production technology is dominated as cis-butenedioic anhydride.With the extensive intensive development of maleic anhydride production, cis-butenedioic anhydride post-processing is increasingly tended to adopt
With solvent absorption-parsing technical matters, typical solvent absorption parsing technique have the graceful technique of Hensel, Conser technique and
ALMA technique, the above two make solvent using dibutyl phthalate (DBP), and the latter uses hexahydrophthalic acid diisobutyl ester
(DIBE) make solvent.Have many research achievements about oxidation technology and absorption parsing technique and be seen in report, Commercial application
Also more steady.
Contain the impurity such as acetic acid, acrylic acid, phthalic anhydride, tar in crude maleic anhydride material after absorbing parsing, wherein acetic acid
It is n butane oxidation by-product with acrylic acid, and phthalic anhydride, tar are then the product of each component cracking, polymerization in resolving, mesh
The acetic acid and acrylic acid that the preceding method for industrially mostly using continuous rectification, first removing boiling point are lower than cis-butenedioic anhydride, then removing recombination
Point, to obtain smart cis-butenedioic anhydride.Acrylic acid in cis-butenedioic anhydride is a kind of thermographic compound, is had on carboxyl site unsaturated double
Key, chemical property are very active.Line is distillated, at overhead condenser in crude maleic anhydride cut light tower rectifying section, tower top, with propylene
The probability of the increase of acid concentration, molecular collision increases, and acrylic acid easily occurs Michael addition reaction and generates dimer and three
Polymers, these oligomer meeting further occurrence Raolical polymerizable generate high molecular polymer, and polymer generated can block up
Pipeline, column plate and the pump housing are filled in, the even running produced to device and technique can cause to seriously affect.In addition, the benzene in crude maleic anhydride
Acid anhydride, tar-like substance are accumulated easily in treating column tower reactor and the coking in tower reactor reboiler, and heat transfer effect is caused to be deteriorated.It is existing
In technology, have using the method for distillating line filling polymerization inhibitor to cut light tower tower top, polymerization inhibitor with acrylic acid by forming surely
Fixed macromolecular compound in subsequent purification tower accumulating and can be tied the macromolecular compound that terminates chain propagation reaction, but generate
Coke causes consequence serious, and usually used polymerization inhibitor is hydroquinone, p-hydroxyanisole or phenthazine.It is inhaled according to solvent
Cis-butenedioic anhydride in the method recycling kettle material of receipts, the macromolecular compound of generation will lead to the increase of solvent processing cost.
Utility model content
In view of the deficiencies of the prior art, the purpose of this utility model is: a kind of crude maleic anhydride continuous rectification apparatus is provided, it can be real
Existing crude maleic anhydride rectifier unit long-period stable operation, and there is design science, structurally reasonable, operating flexibility is big, and economic performance is good
The characteristics of.
Meanwhile the utility model also provides a kind of process using crude maleic anhydride continuous rectification apparatus, scientific and reasonable, letter
It is single easy.
To solve the above problems, technical solution adopted in the utility model are as follows: distributor one end is connected with crude maleic anhydride line,
The other end connect by pipeline with cut light tower, cut light tower top pass through pipeline successively with cut light tower overhead condensation
Device, cut light tower return tank are connected with vacuum system；Cut light tower return tank bottom end by pipeline successively with de- light component
Line is adopted outside tower reflux pump, preheater, mixer, hydrogenator, knockout drum, propionic acid tank, propionic acid pump and propionic acid to connect；Third
Sour pump discharge is connected by pipeline with distributor bottom；Cut light tower bottom end by pipeline successively with cut light tower tower reactor
Pump, treating column, refined tower top condenser, treating column return tank, tail gas washing tower are connected with vacuum system；Tail gas washing tower
Upper end is connect with solvent line, and bottom is successively pumped by pipeline and absorbed with tail gas washing tower tower reactor resolution unit Analytic Tower and connect；
Treating column reflux pot bottom is connected by treating column reflux pump with distributor top；Hydrogenator bottom is provided with regeneration tail
Gas line, gas-liquid separation tank top is provided with plus hydrogen exhaust gas line.
The cut light tower reflux pump is connected by cut light tower return wire with cut light tower upper end；It is de- light
Component tower lower end is provided with cut light tower reboiler；Treating column reflux pump is connected by treating column return wire with treating column upper end
It connects；Treating column one end is provided with smart cis-butenedioic anhydride side and adopts line；It refines tower bottom and successively pumps and absorb solution with treating column tower reactor by pipeline
The connection of unit resolves tower is analysed, treating column lower end is provided with purification tower reboiler；At the top of mixer by pipeline successively with heater
It is connected with hydrogen line, heater is connected with air line and nitrogen line simultaneously.
The cut light tower rectifying section uses sieve tray, and total 4-10 block, every piece of column plate upstream is convex at sloping platform shape
Bubble promoting device, bubble promoting device liquid-facing side do not have bubble holes, carry on the back and are provided with bubble holes on liquid side；Pyramid is provided on sieve pore
Shape calotte, pyramid calotte are made of four pieces of triangle jet trays and one piece of square top plate, and jet tray is equipped with injection
Hole；The spray-hole of adjacent pyramid calotte is on different horizontal planes in horizontal, vertical two orientations.
The position of bubble promoting device is higher than column plate, and the liquid layer on bubble holes is thin, and pressure head is small, carries on the back liquid lateral pressure compared with liquid-facing side
Low, gas is easy to pass through, and forms good bubbling, promotes gas-liquid contact mass transfer, so that liquid phase each component is formed turbulent flow, is overcome with this
Because caused by dead zone or laminar flow the problem of acroleic acid polymerization.In distillation process, liquid on column plate is from calotte bottom gap surrounding
Into in cover, gas then enters in cover from below column plate through sieve pore, by liquid membrane and is ground into many fine drops, gas-liquid
Mixture becomes smaller in uphill process since cross section of fluid channel is long-pending in bubble-cap, generates contracting stream, and pressure energy is partially converted into kinetic energy, makes gas
Liquid mixture flow velocity is accelerated, and the spray-hole on gas-liquid mixture self-injection plate is spouting, rises part after colliding top plate
It turns back, the gas and drop of return are collided with the gas-liquid mixture fierceness of subsequent rising, mixed, the big drop in gas-liquid mixture
It falls after rise into liquid layer, is pressed into cover again through calotte bottom gap and is recycled, and gas then rises to above calotte and rises to
One layer of column plate carries out next step heat transfer, mass transfer, calotte structure becomes gas-liquid two-phase contact mass transfer regional development in cover, cover is outer,
Three spatial dimensions in cover top, and strong disturbance is formed to gas-liquid two-phase, so that plate column column plate space is used for mass transfer entirely, it can be effective
Deadband eliminating or advection slow down acroleic acid polymerization speed, have good anti-organic matter autohemagglutination blocking and solid suspended particle stifled
The ability of plug, overcome operating flexibility existing for traditional float valve tray, small-bore sieve tray it is small, it is easy blocking and large aperture sieve pore
The problem of tower tray mass-and heat-transfer effect difference.The spray-hole cleverly Position Design can effectively eliminate spray-hole work when it is existing
" to spray phenomenon ", avoids entrainment, and reduce energy consumption makes column plate area be fully used, have to improve open ratio of plate
Effect reduces vapor-liquid backmixing on every layer of column plate of knockout tower, reduces gradient of liquid level on every layer of column plate of knockout tower, reduces resistance, improves column plate
Efficiency.
Rectifying section tower tray downspout, column plate bottom surface, the cut light tower tower top of the cut light tower distillate in spool,
Cut light tower tower top cooler and overhead distillate contact portion are each coated with fluorocarbon polymer.
The fluorocarbon polymer is one of polytetrafluoroethylene (PTFE), Kynoar or chlorotrifluoroethylene polymer.It applies
Cover polymer can make covering surface formed a nonwetting surface, make the liquid condensation of polymer easily generated at droplet without
Be adhered on this surface, due to the effect of self gravity, droplet is split away off from surface rapidly because acrylic monomers or
Its oligomer residence time on capped surface is very short, so inhibiting the generation of polymerization reaction.
The cut light tower stripping section uses stainless steel ripple wire packing, and packing layer diameter is 1.5-2.5m, fills out
Bed depth is 2.0-4.0m, and redistributor is arranged at packing layer top, and liquid header is arranged at lower part.Packing layer be located at crude maleic anhydride line with
Below tower body junction, above tower reactor reboiler gaseous line and tower body junction.
Residence time of material can be effectively reduced using stainless steel ripple wire packing, slow down acroleic acid polymerization, in addition, this is filled out
There are also the higher abilities for preventing liquid entrainment mist for material.
The mixer includes fluid passage, gas passage and connector, there is nano-pore on connector, and hydrogen passes through
Nano-pore enters liquid material；The nano-pore aperture is 20-200nm.
Nano-pore disperses gas-liquid two-phase in nano-scale range, to promote acrylic acid and hydrogen in catalyst activity position
Upper absorption improves hydrogenation activity；In addition, acrylic acid hydrogenation is an exothermic reaction, high temperature is easy to cause acroleic acid polymerization, is receiving
Under the action of metre hole, propionic acid, acrylic acid and hydrogen can be completely dispersed in nano-scale range, and acrylic acid is able to effective " isolation ",
It is avoided to polymerize in hydrogenation process.
The treating column is packed tower, and altogether there are three packing layer, packing layer is stainless steel ripple silk net, packing layer diameter
For 2.0-3.5m, the first bed stuffing height is 1.0-2.0m, and the second bed stuffing height is 5.0-7.0m, and third bed stuffing height is
Redistributor is arranged at 1.0-2.0m, each packing layer top, and liquid header is arranged at lower part；Wherein, the first packing layer is located at treating column
Below return wire and tower body junction, adopted above line and tower body junction positioned at smart cis-butenedioic anhydride side；Second packing layer is located at smart cis-butenedioic anhydride
Side is adopted below line and tower body junction, is located above feeding line and tower body junction；Third packing layer is located at feeding line and tower body
Below junction, above purification tower reboiler gaseous line and tower body junction.Select stainless steel ripple packing that can reduce tower pressure drop,
And then bottom temperature is reduced, reduce tar polymerization degree.
The notch diameter of the treating column liquid header is less than filler diameter, can be shortened kettle material and stops in tower reactor
The time is stayed, the generation of polymer is reduced.
The tail gas washing tower is packed tower, and packing layer is stainless steel ripple silk net, and packing layer diameter is 0.5-1.5m,
Bed stuffing height is 1-2m；Redistributor arranged at packing layer top, and liquid header arranged at lower part, packing layer be located at gas-phase feed line with
Above tower body junction, below solvent line and tower body junction.
The cut light tower reboiler, purification tower reboiler all use membrane type reboiler；Cut light tower tower top is cold
Condenser, refined tower top condenser are one of shell and tube or plate heat exchanger.
In view of propionic acid and acrylic acid boiling point and saturated vapour pressure all very close to, but in propionic acid again there is no be easy cause polymerization
Vinyl-functional, therefore utilize this characteristic, propionic acid is added into crude maleic anhydride, the 'inertia' of propionic acid is isolated by acrylic molecules
It opens, to overcome the problem of acrylic acid autohemagglutination.
Cut light tower overhead is propionic acid, acrylic acid, acetic acid and micro cis-butenedioic anhydride.This partial material a part is returned
Stream, a part enters hydrogenator, and in reactor, " reactionlessness " is presented in acetic acid, and because of the reaction position of maleic anhydride hydrogenation
Base is higher, and in hydrogenation reaction, " reactionlessness " is also presented in cis-butenedioic anhydride.Material enters in hydrogenator, in the effect of catalyst
Under, acrylic acid reacts as follows with hydrogen generation:
CH2=CH-COOH+H2→CH3-CH2- COOH (main reaction)；
CH2=CH-COOH+3H2→CH2=CH-CH3+2H2O (side reaction)；
CH2=CH-COOH+4H2→CH3-CH2-CH3+2H2O (side reaction)；
Gas-liquid mixture after reaction enters knockout drum separation, reacts the propylene, propane and unreacted hydrogen of by-product
Gas outlet, liquid product propionic acid return to crude maleic anhydride line and reuse as diluted material.
Process described in the utility model using crude maleic anhydride continuous rectification apparatus, comprising the following steps:
(1) crude maleic anhydride enters cut light tower by distributor along crude maleic anhydride line, utilizes the difference of each component volatility
It is separated, tower system negative pressure is maintained by vacuum system, the light component that tower top obtains is after the condensation of cut light tower overhead condenser
Into cut light tower return tank, phegma after the pressurization of cut light tower reflux pump, return along cut light tower by a part
Streamline returns to cut light tower first layer tower tray, after the preheated device heating of another part, into mixer；Hydrogen is logical in hydrogen line
Enter mixer after crossing heater preheating, mixed with material is adopted outside cut light tower reflux pump, then enter back into hydrogenator,
Under the effect of the catalyst, acrylic acid is reacted with hydrogen, and reaction product enters knockout drum, unreacted hydrogen, propylene, third
For the gases such as alkane along hydrogen exhaust gas line outlet is added, propionic acid enters propionic acid tank along pipeline, and after propionic acid pump pressurization, a part is along third
Line outlet is adopted outside sour, another part returns to distributor along pipeline；
(2) cut light tower materials at bottom of tower enters treating column and further separates, and overhead is condensed through refined tower top
Enter treating column return tank after device condensation, under the action of vacuum system, uncooled gas phase enters tail gas washing tower lower end, molten
Agent enters tail gas washing tower upper end along solvent line, and gas-liquid two-phase counter current contacting in tail gas washing tower is made in the extraction of solvent
Under, the cis-butenedioic anhydride in tail gas enters solvent phase, then after the pump pressurization of tail gas washing tower tower reactor, is adopted outside to absorption resolution unit solution
Analyse tower；For liquid phase in treating column return tank after the pressurization for the treatment of column reflux pump, a part returns to essence along treating column return wire
Tower processed, another part return to distributor；Smart cis-butenedioic anhydride is adopted through smart cis-butenedioic anhydride side and is adopted outside line, and materials at bottom of tower is by the pump pressurization for the treatment of column tower reactor
Afterwards, it adopts outside to absorption resolution unit Analytic Tower；
(3) after hydrogenation reaction carries out a period of time, catalyst can be inactivated because active sites cover, and need regenerated catalyst:
It is firstly introduced into hot nitrogen purging bed, then introduces hot-air, is finally introducing activation gas activated catalyst；Whole process is by adding
Hot device controls temperature of reactor, and purge gass, roasting gas and activation gas are by regeneration tail gas line outlet, and activation finishes backward plus hydrogen is anti-
Introducing raw material and hydrogen in device is answered to be reacted.
In the step 1, the mass ratio of propionic acid and acrylic acid is 20-200:1 at cut light tower feed tray；It is de- light
Component tower top pressure is-100-- 70KPa, and tower bottom pressure is-90-- 60KPa, and cut light tower reflux ratio is 0.7-4:1.
In the step 2, refined tower top pressure is-100-- 70KPa, and tower bottom pressure is-95-- 65KPa；Purification
Tower reflux ratio is 5-20:1.
The cut light tower tower top temperature is 110-140 DEG C, and bottom temperature is 140-170 DEG C；Refined tower top temperature
Degree is 110-130 DEG C, and bottom temperature is 120-140 DEG C；It is 112-132 DEG C that temperature is adopted in treating column side；Tail gas washing tower temperature is
60-80℃；The mass ratio of solvent and cis-butenedioic anhydride in tail gas is 0.2-1:1 in tail gas washing tower.
In hydrogenation process, hydrogen is mixed with acrylic acid, propionic acid by mixer, acrylic acid, hydrogen in hydrogenation process
Molar ratio with propionic acid is 1:1-100:1-100, preferably 1:1-20:10-40.Propionic acid and hydrogen can take away what reaction was released in time
Heat plays the role of " heat carrier ", side reaction caused by capable of effectively avoiding because of high temperature.
The hydrogenation conditions are as follows: reaction pressure 1-2MPa, 40-80 DEG C of reaction temperature, acrylic acid volume space velocity is
0.1-2h-1, the molar ratio of hydrogen and acrylic acid is 1-100:1, preferably 1-20:1 in charging.
Hydrogenation catalyst is loaded catalyst, and active component is in palladium, platinum, nickel, molybdenum or the ruthenium of content 0.2-1wt.%
One or more；Carrier is aluminium oxide or silica, and the specific surface area of catalyst is 50-150m2/ g, aperture 10-50nm.
In the step 3, purging temperature is 60-200 DEG C, and maturing temperature is 300-400 DEG C.The new agent of catalyst or regeneration
The active component of catalyst afterwards is oxidation state, needs to draw also Primordial Qi activated catalyst before reaction, activation gas be hydrogen or hydrogen/
One of nitrogen mixture；Activation temperature is 200-350 DEG C, activation pressure 0-0.2MPa, and hydrogen volume air speed is 1000-
1500h-1。
Treating column kettle material group becomes cis-butenedioic anhydride and heavy constituent, this partial material, which returns, absorbs resolution unit Analytic Tower, benefit
With the different separation cis-butenedioic anhydrides and heavy constituent of boiling point, higher boiling coke oil compounds enter solvent phase, then through solvent processing unit
Removing.
Material in treating column tower reactor extraction line, which enters, absorbs resolution unit Analytic Tower, by reducing bottom temperature, improving
The method that treating column tower reactor produces the amount of adopting outside line reduces bottom temperature, shortens in kettle material tar in the residence time of tower reactor,
Reduce the generation of coking material.
Compared with prior art, the utility model has the following beneficial effects:
1. crude maleic anhydride continuous rectification apparatus described in, design science is structurally reasonable, is able to achieve crude maleic anhydride rectifier unit long week
Phase stable operation has the advantages that operating flexibility is big, economic performance is good；Acrylic acid can also be effectively overcome to hang stifled, tar coking
Problem, and distillation process will not secondary pollution cis-butenedioic anhydride, obtained smart yield of maleic anhydride is high, purity is high.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of crude maleic anhydride continuous rectification apparatus；
Fig. 2 is the tower plate structure schematic diagram of sieve tray；
Fig. 3 is the structural schematic diagram of pyramid calotte；
Fig. 4 is the overlooking structure diagram of pyramid calotte；
In figure, 1- crude maleic anhydride line；2- distributor；3- cut light tower；4- cut light tower tower reactor pump；5- cut light tower
Overhead condenser；6- cut light tower return tank；7- cut light tower return tank；8- cut light tower reboiler；9- takes off light group
Divide tower reflux pump；10- preheater；11- regeneration tail gas line；12- air line；13- nitrogen line；14- hydrogen line；15- heater；
16- mixer；17- hydrogenator；18- knockout drum；19- adds hydrogen exhaust gas line；20- propionic acid tank；21- propionic acid pump；22- third
Line is adopted outside sour；23- treating column；24- refined tower top condenser；25- treating column return tank；26- treating column reflux pump；27- essence
Tower return wire processed；Adopt line in 28- essence cis-butenedioic anhydride side；29- refines tower reboiler；30- treating column tower reactor pump；31- tail gas washing tower；32-
Tail gas washing tower tower reactor pump；33- absorbs resolution unit Analytic Tower；34- vacuum system；35- solvent line；36- cut light tower tower
Body；37- bubble holes；38- bubble promoting device；39- pyramid calotte；40- downspout；41- sieve pore；42- column plate；43- top plate；
44- jet tray；45- spray-hole.
Specific embodiment
Explanation and embodiment are described further the utility model with reference to the accompanying drawing.
Embodiment 1
The crude maleic anhydride continuous rectification apparatus, 2 one end of distributor are connected with crude maleic anhydride line 1, the other end by pipeline with
Cut light tower 3 connects, at the top of cut light tower 3 by pipeline successively with cut light tower overhead condenser 5, cut light tower
Return tank 6 and vacuum system 34 connect；6 bottom end of cut light tower return tank by pipeline successively with cut light tower reflux pump 9,
Preheater 10, mixer 16, hydrogenator 17, knockout drum 18, propionic acid tank 20, propionic acid pump 21 and the outer line 22 of adopting of acid connect
It connects；21 outlet of acid pump is connected by pipeline with 2 bottom of distributor；3 bottom end of cut light tower by pipeline successively with take off light group
Divide tower tower reactor pump 4, treating column 23, refined tower top condenser 24, treating column return tank 25, tail gas washing tower 31 and vacuum system
34 are connected；31 upper end of tail gas washing tower is connect with solvent line 35, and bottom successively pumps 32 with tail gas washing tower tower reactor by pipeline
It is connected with resolution unit Analytic Tower 33 is absorbed；25 bottom for the treatment of column return tank passes through 2 top for the treatment of column reflux pump 26 and distributor
It is connected；17 bottom of hydrogenator is provided with regeneration tail gas line 11, and gas-liquid separation tank top is provided with plus hydrogen exhaust gas line 19.
The cut light tower reflux pump 9 is connected by cut light tower return wire 7 with 3 upper end of cut light tower；
Cut light tower lower end is provided with cut light tower reboiler 8；Treating column reflux pump 26 passes through treating column return wire 27 and purification
23 upper end of tower is connected；23 one end for the treatment of column is provided with smart cis-butenedioic anhydride side and adopts line 28；23 bottom for the treatment of column by pipeline successively with essence
Tower tower reactor pump 30 processed is connected with resolution unit Analytic Tower is absorbed, and treating column lower end is provided with purification tower reboiler 29；Mixer 16
Top is successively connect with heater 15 and hydrogen line 14 by pipeline, and heater 15 is connected with air line 12 and nitrogen line 13 simultaneously
It connects.
The rectifying section of the cut light tower 3 uses sieve tray, and total 4-10 block, every piece of 42 upstream of column plate is convex at oblique
Mesa-shaped bubble promoting device 38,38 liquid-facing side of bubble promoting device do not have bubble holes 37, carry on the back and are provided with bubble holes 37 on liquid side；Sieve pore 41
On be provided with pyramid calotte 39, pyramid calotte 39 is by four pieces of triangle jet trays 44 and one piece of square top plate 43
It constitutes, jet tray 44 is equipped with spray-hole 45；The spray-hole 45 of adjacent pyramid calotte 39 in horizontal, vertical two orientations
On different horizontal planes.
Rectifying section tower tray downspout, column plate bottom surface, the cut light tower tower top of the cut light tower distillate in spool,
Cut light tower tower top cooler and overhead distillate contact portion are each coated with polytetrafluoroethylene (PTFE).
The stripping section of cut light tower uses stainless steel ripple wire packing, and packing layer diameter is 1.5m, bed stuffing height
For 2.0m, filler is stainless steel ripple silk net.Redistributor is arranged at the packing layer top, and liquid header, filler are arranged at lower part
Layer is located at below crude maleic anhydride line 1 and tower body junction, above tower reactor reboiler gaseous line and tower body junction.
The treating column 23 is packed tower, and altogether there are three packing layer, packing layer is stainless steel ripple silk net, and packing layer is straight
Diameter is 2.0-3.5m, and the first bed stuffing height is 1.0-2.0m, and the second bed stuffing height is 5.0-7.0m, third bed stuffing height
For 1.0-2.0m, redistributor is arranged at each packing layer top, and liquid header is arranged at lower part；Wherein, the first packing layer is located at purification
Below tower return wire 27 and tower body junction, adopted above line 28 and tower body junction positioned at smart cis-butenedioic anhydride side；Second packing layer is located at
Smart cis-butenedioic anhydride side is adopted below line 28 and tower body junction, is located above feeding line and tower body junction；Third packing layer is located at charging
Below line and tower body junction, above purification 29 gaseous line of tower reboiler and tower body junction.Treating column liquid collection trough diameter
Less than filler diameter.
The mixer 16 includes fluid passage, gas passage and connector, there is nano-pore on connector, and hydrogen is logical
It crosses nano-pore and enters liquid material, the aperture of nano-pore is 20nm.
The cut light tower reboiler 8 and purification tower reboiler 29 uses membrane type reboiler, cut light tower tower top
Condenser 5 and refined tower top condenser 24 are tubular heat exchanger.
The tail gas washing tower 31 is packed tower, and filler is stainless steel ripple silk net, and packing layer diameter is 0.5-1.5m,
Bed stuffing height is 1-2m；Redistributor arranged at packing layer top, and liquid header arranged at lower part, packing layer be located at gas-phase feed line with
Above tower body junction, below solvent line 35 and tower body junction.
The crude maleic anhydride material composition for carrying out self-absorption resolution unit is as shown in table 1；Propionic acid is added in cut light tower, is passed through
It adjusts, makes to enter the mass ratio 20:1 of the propionic acid and acrylic acid at cut light tower feed column column plate, material is formed such as 2 institute of table
Show:
1 crude maleic anhydride material of table composition
| Ingredient | H2O | Acetic acid | Acrylic acid | Cis-butenedioic anhydride | Heavy constituent |
| It forms (wt.%) | 0.10 | 0.30 | 1.20 | 98.30 | 0.10 |
The material that table 2 enters cut light tower forms
| Ingredient | H2O | Acetic acid | Propionic acid | Acrylic acid | Cis-butenedioic anhydride | Heavy constituent |
| It forms (wt.%) | 0.08 | 0.24 | 19.40 | 0.97 | 79.23 | 0.08 |
The process using crude maleic anhydride continuous rectification apparatus, includes the following steps:
(1) crude maleic anhydride material enters cut light tower 3 by distributor 2 along crude maleic anhydride line 1, boils again in cut light tower
It under the thermal drivers effect of device 8, is separated using the difference of each component volatility, tower system negative pressure, tower is maintained by vacuum system 34
It pushes up obtained light component and enters cut light tower return tank 6 after the condensation of cut light tower overhead condenser 5, phegma is by de-
After lights column reflux pump 9 pressurizes, a part returns to 3 first layer tower tray of cut light tower along cut light tower return wire, separately
After a part of preheated device 10 heats, into mixer 16；Cut light tower tower top pressure be -70KPa, tower bottom pressure be -
60Kpa, tower top temperature are 110 DEG C, and bottom temperature is 140 DEG C, reflux ratio 4.Hydrogen is pre- by heater 15 in hydrogen line 14
Enter mixer 16 after heat, is mixed with material is adopted outside cut light tower reflux pump 9, then enter back into hydrogenator 17, urging
Under the action of agent, acrylic acid is reacted with hydrogen, and reaction product enters knockout drum 18, unreacted hydrogen, propylene, propane
For equal gases along 19 outlet of hydrogen exhaust gas line is added, propionic acid enters propionic acid tank 20 along pipeline, after 21 pressurization of propionic acid pump, a part of edge
22 outlet of line is adopted outside propionic acid, another part returns to distributor 2 along pipeline；Wherein, hydrogenation conditions are as follows: reaction pressure
2Mpa, 40 DEG C of reaction temperature, acrylic acid volume space velocity is 2h-1, the molar ratio of hydrogen and acrylic acid is 20 in charging；Hydrogenation catalyst
Agent is loaded catalyst, and active component is palladium, and catalyst carrier is silica, and active component content amounts to 1wt%, catalyst
Specific surface area be 50m2/ g, aperture 50nm.At this point, acrylic acid conversion ratio is 99.8%, product propionic acid is selectively
99.5%.
After separation, cut light tower overhead, bottoms group material composition are as shown in table 3, table 4:
3 cut light tower overhead of table composition
| Ingredient | Acetic acid | Propionic acid | Acrylic acid | Cis-butenedioic anhydride |
| It forms (wt.%) | 1.14 | 92.38 | 4.62 | 0.23 |
4 cut light tower materials at bottom of tower of table composition
| Ingredient | Propionic acid | Acrylic acid | Cis-butenedioic anhydride | Heavy constituent |
| It forms (wt.%) | 0.20 | 0.02 | 99.66 | 0.12 |
(2) 3 materials at bottom of tower of cut light tower enters treating column 23 and further separates, and overhead is cold through refined tower top
Condenser 24 enters treating column 25 after condensing, and under the action of vacuum system 34, uncooled gas phase enters under tail gas washing tower 31
End, solvent enter 31 upper end of tail gas washing tower, gas-liquid two-phase counter current contacting in tail gas washing tower 31, molten along solvent line 35
Under the extraction of agent, the cis-butenedioic anhydride in tail gas enters solvent phase, then after 32 pressurization of tail gas washing tower tower reactor pump, is adopted outside to suction
Receive resolution unit Analytic Tower 33；Liquid phase in treating column return tank 25 after the pressurization for the treatment of column reflux pump 26, a part along
Treating column return wire 27 returns to treating column 23, and another part returns to distributor 2；Smart cis-butenedioic anhydride is adopted through smart cis-butenedioic anhydride side and is adopted outside line 28, tower
Substrate material is adopted outside after 30 pressurization for the treatment of column tower reactor pump to absorption resolution unit Analytic Tower 33；Wherein, 23 tower top pressure for the treatment of column
Power is -70KPa, and tower bottom pressure is -65KPa, and tower top temperature is 110 DEG C, and bottom temperature is 120 DEG C, and it is 112 DEG C that temperature is adopted in side,
Treating column reflux ratio is 5；Tail gas washing tower temperature is 60 DEG C, and cis-butenedioic anhydride mass ratio is 0.2 in solvent and tail gas, at this point, in tail gas
Recovery of Maleic Anhydride rate is 99.9%.
(3) after hydrogenation reaction carries out a period of time, catalyst can be inactivated because active sites cover, and need regenerated catalyst:
It is firstly introduced into hot nitrogen purging bed, then introduces hot-air, is finally introducing activation gas activated catalyst；Whole process is by adding
Hot device controls temperature of reactor, and purge gass, roasting gas and activation gas are by regeneration tail gas line outlet, and activation finishes backward plus hydrogen is anti-
Introducing raw material and hydrogen in device is answered to be reacted.
In step 3, purging temperature is 100 DEG C, and maturing temperature is 350 DEG C.
The active component of catalyst after the new agent of catalyst or regeneration is oxidation state, needs to draw also Primordial Qi activation before reaction and urges
Agent, activation gas is hydrogen；Activation temperature is 200 DEG C, and activation pressure is -0.2MPa, and hydrogen volume air speed is 1500h-1。
After separation, refined tower top distillate, treating column production composition are respectively as shown in table 5,6,7:
5 refined tower top distillate of table composition
| Ingredient | Propionic acid | Acrylic acid | Cis-butenedioic anhydride |
| It forms (wt.%) | 0.21 | 0.02 | 99.77 |
Adopt production composition in 6 treating column side of table
| Ingredient | Cis-butenedioic anhydride |
| It forms (wt.%) | 99.92 |
7 treating column tower reactor production of table composition
| Ingredient | Cis-butenedioic anhydride | Heavy constituent |
| It forms (wt.%) | 99.88 | 0.12 |
In the present embodiment, device continuous and stable has been run 10 months, and cut light tower tower pressure difference maintains 10-20KPa, is not had
Have and big fluctuation occurs, tower top, tower bottom production composition are steady, this illustrates cut light tower column plate, and there is no acrylic acid extensions
It is stifled, do not influence heat and mass.Treating column tower bottom reboiler heating medium flow is stablized, and there is no because of tar class object for this explanation
The problem of tower reboiler heat-transfer effect difference is refined caused by matter coking.
Hydrogenator operation cycle is 8 months.
Claims (5)
1. a kind of crude maleic anhydride continuous rectification apparatus, it is characterised in that: distributor (2) one end is connected with crude maleic anhydride line (1), the other end
Connect by pipeline with cut light tower (3), at the top of cut light tower (3) by pipeline successively with cut light tower overhead condensation
Device (5), cut light tower return tank (6) and vacuum system (34) connection；Cut light tower return tank (6) bottom end by pipeline according to
It is secondary with cut light tower reflux pump (9), preheater (10), mixer (16), hydrogenator (17), knockout drum (18),
Line (22) connection is adopted outside propionic acid tank (20), propionic acid pump (21) and propionic acid；Propionic acid pumps (21) outlet and passes through pipeline and distributor (2) bottom
Portion is connected；Cut light tower (3) bottom end successively pumps (4), treating column (23), treating column with cut light tower tower reactor by pipeline
Overhead condenser (24), treating column return tank (25), tail gas washing tower (31) are connected with vacuum system (34)；Tail gas washing tower
(31) upper end is connect with solvent line (35), and bottom is successively pumped (32) with tail gas washing tower tower reactor by pipeline and absorbs resolution unit
Analytic Tower (33) connection；Treating column return tank (25) bottom at the top for the treatment of column reflux pump (26) and distributor (2) by being connected；
Hydrogenator (17) bottom is provided with regeneration tail gas line (11), is provided at the top of knockout drum (18) and is added hydrogen exhaust gas line
(19)。
2. crude maleic anhydride continuous rectification apparatus according to claim 1, it is characterised in that: cut light tower reflux pump (9) is logical
Cut light tower return wire (7) is crossed to connect with cut light tower (3) upper end；Cut light tower (3) lower end is provided with de- light component
Tower reboiler (8)；Treating column reflux pump (26) is connect by treating column return wire (27) with treating column (23) upper end；Treating column
(23) one end is provided with smart cis-butenedioic anhydride side and adopts line (28)；Treating column (23) bottom by pipeline successively with treating column tower reactor pump (30) and
Resolution unit Analytic Tower (33) connection is absorbed, treating column (23) lower end is provided with purification tower reboiler (29)；Mixer (16) top
Portion is successively connect by pipeline with heater (15) and hydrogen line (14), heater (15) and meanwhile with air line (12) and nitrogen line
(13) it is connected.
3. crude maleic anhydride continuous rectification apparatus according to claim 1, it is characterised in that: the rectifying section of cut light tower (3)
Using sieve tray, total 4-10 block, every piece of column plate (42) upstream is convex at sloping platform shape bubble promoting device (38), bubble promoting device
(38) liquid-facing side does not have bubble holes (37), carries on the back and is provided with bubble holes (37) on liquid side；Sieve pore is provided with pyramid cap on (41)
It covers (39), pyramid calotte (39) is made of four pieces of triangle jet trays (44) and one piece of square top plate (43), is sprayed
Plate (44) is equipped with spray-hole (45)；The spray-hole (45) of adjacent pyramid calotte (39) in horizontal, vertical two orientations
On different horizontal planes.
4. according to crude maleic anhydride continuous rectification apparatus described in claim 1, it is characterised in that: treating column (23) is packed tower, is shared
Three packing layers, packing layer are stainless steel ripple silk net, and packing layer diameter is 2.0-3.5m, and the first bed stuffing height is 1.0-
2.0m, the second bed stuffing height are 5.0-7.0m, and third bed stuffing height is 1.0-2.0m, and redistribution is arranged at each packing layer top
Liquid header is arranged at device, lower part.
5. crude maleic anhydride continuous rectification apparatus according to claim 1, it is characterised in that: tail gas washing tower (31) is filler
Tower, packing layer are stainless steel ripple silk net, and packing layer diameter is 0.5-1.5m, bed stuffing height 1-2m；Packing layer top has
Liquid header is arranged at redistributor, lower part.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109761940A (en) * | 2019-03-18 | 2019-05-17 | 淄博齐翔腾达化工股份有限公司 | Crude maleic anhydride continuous rectification apparatus and process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109761940A (en) * | 2019-03-18 | 2019-05-17 | 淄博齐翔腾达化工股份有限公司 | Crude maleic anhydride continuous rectification apparatus and process |
| CN109761940B (en) * | 2019-03-18 | 2024-03-26 | 淄博齐翔腾达化工股份有限公司 | Continuous rectifying device and process method for crude maleic anhydride |
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