CN104109088A - Sec-butyl acetate production line - Google Patents
Sec-butyl acetate production line Download PDFInfo
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- CN104109088A CN104109088A CN201410279570.9A CN201410279570A CN104109088A CN 104109088 A CN104109088 A CN 104109088A CN 201410279570 A CN201410279570 A CN 201410279570A CN 104109088 A CN104109088 A CN 104109088A
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Abstract
The invention discloses a sec-butyl acetate production line, which includes an esterification reaction system, a separation refining system and an acetic acid recovery system. The outlet end of the esterification reaction system is connected to the inlet end of the separation refining system. The acetic acid outlet end of the separation refining system is connected to the inlet end of the acetic acid recovery system, which is in connection with the esterification reaction system. The production line provided by the invention can realize real-time control of the whole production process, and excessive acetic acid in the product separation refining and esterification reaction can be recycled, thus saving resources. The production line can control the reaction temperature in each reactor, can reduce the corrosion of water containing acetic acid on equipment and pipelines, prolongs the life of the catalyst, and also can perform effective alkali washing on all equipment tail gas, thus preventing corrosion and environment pollution.
Description
Technical field
The present invention relates to a kind of 2-butyl acetate production unit, be specifically related to a kind of 2-butyl acetate production line.
Background technology
At present, 2-butyl acetate is mainly as solvent, chemical reagent, grease, resin, coating, paint etc., in recent years due to the raising of environmental requirement, use containing noxious solvents such as benzene, toluene is restricted just gradually, the consumption of acetates environmentally friendly solvent sharply increases, so 2-butyl acetate has wide market, builds new 2-butyl acetate device imperative.The outstanding feature that acid esters is combined to 2-butyl acetate technique is to adopt cheap refinery's by product---mixed c 4, utilizes the butene component in C4 resource, the direct and acetic acid synthesized secondary butyl ester of acetic acid esterified under catalyst action.But a lot of problem of existence that the traditional processing technology of 2-butyl acetate exists, especially continuous refining route is long, and investment is large, and production cost is high, excessive acetic acid in the refining and esterification of product separation can not recycle in whole production technique system, causes the wasting of resources etc.
Summary of the invention
Object of the present invention is exactly the defect existing for prior art, provide a kind of and can control in real time, product separation is refining and esterification in excessive acetic acid can recycle, economize on resources, can control the temperature of reaction in each reactor, can reduce the corrosion of water-containing acetic acid to equipment, pipeline, the extending catalyst life-span, can carry out effective alkali cleaning to each equipment tail gas, prevent the 2-butyl acetate production line of corrosion and contaminate environment.
Its technical scheme is: 2-butyl acetate production line, comprises esterification system, separation and purification system and acetic acid recovery system; The exit end of described esterification system is connected with the inlet end of separation and purification system, and the acetic acid exit end of described separation and purification system is connected with the inlet end of acetic acid recovery system, and described acetic acid recovery system is connected with esterification system;
Described esterification system comprises C 4 olefin head tank, coalescer, carbon four strainers, esterifier, acetate buffer tank, acetic acid fresh feed pump, acetic acid cleaner and acetic acid preheater, and described C 4 olefin head tank is connected with mixer entrance with carbon four strainers by coalescer; Described acetate buffer tank is connected with acetic acid cleaner through acetic acid fresh feed pump, and the outlet of acetic acid cleaner is connected with acetic acid preheater inlet end, and described acetic acid preheater is connected with mixer entrance, and described mixer outlet is connected with esterifier;
Described separation and purification system comprises decarburization four devices, azeotropic distillation device, depickling reaction unit and acetic acid refining device; Described decarburization four devices comprise decarburization four towers that are connected with esterifier outlet, described decarburization four towers are connected with decarburization four overhead condensers by decarburization four tower reflux pumps through decarburization four tower return tanks, on decarburization four towers, be also connected with decarburization four tower reboilers and carbon four water wash columns, the top of carbon four water wash columns is connected with washing carbon four surge tanks; Described azeotropic distillation device comprises and the azeotropy rectification column being connected at the bottom of decarburization four tower towers, the tower top of azeotropy rectification column is connected with azeotropic overhead condenser by azeotropy rectification column return tank, the tower top of azeotropy rectification column is connected with carbon four water wash columns, the inlet end of azeotropy rectification column is also connected with fresh acetic acid feed line and greasy dirt transferpump, azeotropy rectification column is provided with transferpump at the bottom of azeotropic tower bottom reboiler and tower, and at the bottom of tower, transferpump is connected with acetic acid refining device by thick acetic acid line of pipes; Described depickling reaction unit comprises thick ester depickling reactor and the ester product tower being connected with azeotropy rectification column by layering ester phase transferpump, ester product tower is connected with ester product condenser, ester product tower bottom reboiler and ester product reflux tank, on the pipeline of thick ester depickling reactor and ester product tower, ester product tower feed exchanger is installed, ester reactor product cooler is connected with ester product tower feed exchanger, ester product tower feed exchanger is connected with ester product surge tank, and ester product tower bottom reboiler is provided with heavies water cooler; Described acetic acid refining device comprises the acetic acid refining tower being connected with azeotropy rectification column, is connected with acetic acid refining tower tower bottom reboiler, acetic acid refining column overhead condenser, acetic acid refining tower return tank and the acetate buffer tank being connected with acetic acid refining tower reflux pump on acetic acid refining tower in turn;
Described acetic acid recovery system comprises and being connected with acetic acid refining tower and the tank connected acetic acid refining tower of acetate buffer reflux pump.
Described esterification system also comprises the chain logic device being arranged in esterification pipeline.
Described esterifier is shell and tube reactor.
Described mixing tank comprises carbon four mixing tanks of two series connection.
The present invention compared with prior art, have the following advantages: can control in real time whole production technique, product separation is refining and esterification in excessive acetic acid can recycle, economize on resources, can control the temperature of reaction in each reactor, can reduce the corrosion of water-containing acetic acid to equipment, pipeline, the extending catalyst life-span, and can carry out effective alkali cleaning to each equipment tail gas, prevent corrosion and contaminate environment.
Accompanying drawing explanation
Fig. 1 is technological process of production schematic diagram of the present invention;
Fig. 2 is the process flow diagram of esterification system;
Fig. 3 is the process flow diagram of decarburization four devices;
Fig. 4 is the process flow diagram of azeotropic distillation device;
Fig. 5 is the process flow diagram of depickling reaction unit;
Fig. 6 is the process flow diagram of acetic acid refining device;
Fig. 7 is hot water circulation artwork;
Fig. 8 is washing tail gas artwork;
Wherein:
Carbon four preheaters 1, coalescer 2, carbon four strainers 3, C 4 olefin head tank 4, acetate buffer tank 5, acetic acid fresh feed pump 6, acetic acid cleaner 7, acetic acid preheater 8, mixing tank 9, the first carbon four mixing tanks 91, the second carbon four mixing tanks 92, esterifier 10, spinner-type flowmeter 11, chain logical one 2, reactor product tank 13, reflux pump 14, carry carbon four raw material pipelines 15, steam condensation water tank 16, vapor can 17, decarburization four tower reboilers 18, decarburization four towers 19, transport pipe 20, decarburization four overhead condensers 21, decarburization four tower return tanks 22, carbon four washing towers 23, washing carbon four surge tanks 24, carbon four transferpumps 25, layering water tank 26, sewage compounding substances tank 27, layering ester is to transferpump 28, layering aqueous-phase reflux pump 29, thick acetic acid line of pipes 30, at the bottom of tower, transferpump 31, azeotropic tower bottom reboiler 32, fresh acetic acid feed line 33, decarburization four bottoms line of pipes 34, azeotropy rectification column 35, azeotropic overhead condenser 36, desalting pipe netting twine 37, signal source 38, azeotropy rectification column return tank 39, ester product tower reflux pump 40, ester tower return tank water transferpump 41, ester product surge tank 42, 2-butyl acetate transferpump 43, thick ester depickling reactor 44, ester reactor product cooler 45, ester product tower feed exchanger 46, ester product tower bottom reboiler 47, ester product tower 48, ester product tower condenser 49, ester product tower return tank 50, heavies transferpump 51, heavies surge tank 52, heavies alkali cleaning buffering pump 53, heavies alkali cleaning water cooler 54, heavies alkali cleaning fresh feed pump 55, heavies water cooler 56, acetic acid refining tower tower bottom reboiler 57, acetic acid refining tower 58, acetic acid refining column overhead condenser 59, acetic acid refining tower return tank 60, acetic acid refining tower reflux pump 61, heavies alkali cleaning layering tank 62, hot recycle pump 63, hot water basin 64, hot water cooler 65, tail gas alkali recycle pump 66, tail gas alkali cleaning of evaporator 67, dense acetic acid emptying device 68, acetate in minute emptying device 69, tail gas divides flow container 70, alkali solution cooler 71, sump oil transferpump 72, sump oil basin 73, hot-water line 74.
Embodiment
The present invention is comprised of two process systems in production technique, and a kind of is esterification system: the n-butene in material carbon four and excessive acetic acid is acetic acid synthesized secondary butyl ester under resin catalyst effect; The 2nd, product separation refining system: the excessive acetic acid by 2-butyl acetate product separation in refining and esterification recycles in native system.
As depicted in figs. 1 and 2, C 4 olefin raw material is sent into from C 4 olefin head tank 4, after coalescer 3, carbon four strainer 2 separated free water, sends into carbon four preheaters 1 and is heated to 70---100 ℃, then divides four stock materials under flow control, to enter carbon four mixing tanks 9.
On conveying C 4 olefin raw material pipeline, temperature indicating instrument is installed and is connected with signal wire with room temp indicating controller table, the temperature in major control feed line road, simultaneously installing analysis sample apparatus on pipeline.
Acetic acid raw material is from acetate buffer tank 5, get and send into acetic acid cleaner 7 through acetic acid fresh feed pump 6, acetic acid cleaner 7 is two purifier devices in parallel, sorbent material is inside housed to remove metallic cation, after two cleaner operation for some time inefficacies, switches and more renew agent.Acetic acid after purification enters acetic acid preheater 8 and is heated to 100 ℃ of 60-and enters the first carbon four mixing tanks 91 under flow control, after acetic acid and carbon four mix, enters the second mixing tank 92, after then mixing with carbon four, enters esterifier 10.In this process, wherein some carbon four-function is crossed spinner-type flowmeter 11, is entered esterifier 10.Esterifier 10 is shell and tube reactor, is respectively I, II, III, IV, filling esterification resin catalyst in pipe, and shell side passes into circulating hot water and carries out heat-obtaining; Reaction product enters I, II, III, the heat release of IV esterification reaction process of esterifier 10 successively after mixing with fresh carbon four, by controlling temperature and the flow of shell side circulating hot water, to guarantee that esterifier I, II, III, IV approach isothermal reaction.Esterification requires to carry out under full liquid-phase condition, so reaction pressure controlled by the IV top hole pressure of esterifier 10, and the IV top hole pressure of esterifier 10 is controlled at 1.5MPaG.Reaction product enters decarburization four towers 19 after pressure controlled valve step-down.
Chain logic device 12 is arranged on whole 2-butyl acetate and produces on main position, guarantees that whole state of the art monitors enforcement.
Acetic acid preheater 8 top and bottom are provided with Safety control valve, top Safety control valve setting pressure indicating controller table and pressure-controlling alarming instrument, the Safety control valve that install bottom is mainly effectively to control to discharge the solidifying water generating after partial heat energy, be arranged on pressure controlled valve under acetic acid preheater 8 by electromotive signal line with after four mixing of first strand of carbon, enter the temperature control instrument that esterifier 8 is arranged on conveying pipeline and be connected.
Setting pressure safety instrument being connected with pressure-controlling instrument by electromotive signal line on the transport pipe between mixing tank 92 and esterifier 10, all setting pressure safety instrument and pressure-controlling instrument on the transport pipe between the II of mixing tank and esterifier 10, III, IV.
The I of esterifier 10, II, III discharge partially aqueous acetic acid, enter sump oil basin 72; Product introduction decarburization four towers 19 of the IV reaction of esterifier 10.Flow valve 13 and flow control instrument are installed on transport pipe, and have electromotive signal line to connect.
As shown in Figure 3, reaction product enters decarburization four towers 19 by transport pipe 20, and the object of decarburization four towers 19 is that unreacted carbon four in esterification is separated with last running such as acetic acid, SBA, carbon eight alkene, carbon benzenes.Unreacted a part of product introduction carbon four water wash columns 23, carbon four water wash columns 23 are liquid-liquid extraction tower, object is washed the acetic acid water of trace in carbon four off, to meet liquefied gas quality and line of pipes and equipment corrosion requirement.Come pipe network 1.5Mpa vapor can 17, enter decarburization four tower reboilers 18, the four tower reboiler 18 release portion steam condensation waters of decarburization simultaneously enter steam condensation water tank 16, on decarburization four tower reboilers 18, setting pressure control instruments is connected with signal wire with the pressure-controlling instrument being arranged on the solidifying waterpipe of released vapour, and has chain.
Portioned product in decarburization four towers 19 enters decarburization four tower reboilers 18 through piping, use 1.5MPaG steam heating, tower top carbon four is for bubble point condensation and take hot vapor bypass control, carbon four liquid are through decarburization four tower reflux pumps 14, part carbon four liquid are through decarburization four tower reflux pumps 14, through decarburization four tower return tanks 22, decarburization four overhead condensers 21 are done to reflux and are delivered to decarburization four tower 19 tower tops, and directly with through decarburization four tower return tanks 22 are connected without decarburization four overhead condensers 21 by pipeline.A part is sent into carbon four water wash columns 23, and carbon four water wash columns 23 are connected with layering water tank 26.Decarburization four tower 19 bottomss enter azeotropy rectification column 35 by tower self-pressure under tower reactor liquid level and the control of extraction flow tandem.Decarburization four tower return tanks 22 are installed air emptying pipeline.Carbon four-way is crossed conveying carbon four raw material pipelines 15 and is exported by decarburization four tower 19 bottoms.
The product of sending into carbon four water wash columns 23 contains sewage and acetic acid water, a part is that layering water is from layering aqueous-phase reflux pump 29, a part enters azeotropy rectification column 35 through sewage mixing duct 27, carbon four water wash column 23 top products enter washing carbon four surge tanks 24 by pipeline, carbon four water wash columns 23 must have certain temperature and pressure, temperature 40-50 ℃, pressure 0.5-1Mpa, and temperature control instrument and pressure-controlling instrument be installed, by pipeline, enter washing carbon four surge tanks 24 and also have certain temperature and pressure, temperature is 40 ℃ of left and right, pressure 0.5Pma, temperature control instrument is installed, pressure-controlling instrument, right part at washing carbon four surge tanks 24 is installed liquid level controller table, emptying gas pipeline is installed on washing carbon four surge tank 24 tops, emptying sewer pipeline is installed in bottom, inside is product carbon four.
From the water of azeotropy rectification column 35, through layering aqueous-phase reflux pump 29, send into carbon four water wash columns 23 and enter carbon four counter current contact containing acetate in minute, at the bottom of tower, acid-bearing wastewater returns to azeotropy rectification column 35, by layering ester, to transferpump 28, azeotropy rectification column 35 is steamed to layering ester product and be back to azeotropy rectification column 35 by azeotropy rectification column return tank 39, carbon four water wash columns 23 are packing tower, in tower, carbon four is disperse phase, water is external phase, by controlling the position, boundary of carbon four and water, to guarantee that water and carbon four contact well in filler, also guarantee the settlement separate of carbon four and water simultaneously.Control hierarchy discharge, to guarantee that carbon four washings reach requirement.The carbon four that tower top flows out enters washing carbon four surge tanks 24, further removes the free-water carrying, and working pressure is bubbling pressure, and the carbon four after minute water is delivered to tank field liquefied gas storage through carbon four transferpumps 25.
As shown in Figure 4, come the fresh acetic acid feed line 33 of pipe network, come decarburization four tower product substrate line of pipes 34, the profit of carrying with sump oil transferpump 71 enters azeotropy rectification column 35.Azeotropy rectification column 35 is adopted and is used water as entrainer, by azeotropic distillation mode, acetic acid is separated with 2-butyl acetate, carbon eight alkene etc., tower top obtains the thick ester containing a small amount of carbon eight alkene and carbon benzene, at the bottom of tower, be the acetic acid containing last running such as a small amount of 2-butyl acetate, carbon benzenes, the water that return tank of top of the tower 22 multi_layer extractions go out all refluxes.In azeotropy rectification column 35, because acetic acid exists, 2-butyl acetate is hydrolyzed on a small quantity, generate sec-butyl alcohol and acetic acid, sec-butyl alcohol and water form minimum azeotrope, by tower top, with 2-butyl acetate, water, are together steamed.Fresh acetic acid raw material contains a small amount of water (about 2000ppm) and metallic cation, metallic cation can make catalysts poisoning and deactivation, and water and olefine reaction can produce alcohol, therefore for reducing side reaction, reduce the corrosion of water-containing acetic acid to equipment, pipeline simultaneously, therefore in the extending catalyst life-span, fresh acetic acid is sent into azeotropy rectification column 35 dewaters, demetalization positively charged ion.
The blow-down pipe of azeotropy rectification column return tank 39 is connected with torch pipe network, and the about 30KPa of working pressure, is connected with desalting pipe netting twine 37 on azeotropy rectification column return tank 39, on azeotropy rectification column return tank 39, liquid level indicator instrument is installed, and is connected with signal source 38.
Ester product tower return tank 50 is used 1.0MPa steam heating.Ester product tower return tank 50 is used 1.0MPa steam heating.The 2-butyl acetate that tower top steams, carbon eight, water etc., through condensing cooling to 45～60 ℃, enter layering in carbon four water wash columns 23, and water is returned stream through layering aqueous-phase reflux pump 29 parts, another part carbon elimination four water wash column 23 washing unreacted carbon four.Oil phase is returned stream through layering ester phase transferpump 28 parts, and another part is squeezed into thick ester depickling reactor 44.Because layering tank median water level can reduce gradually, can be by de-mineralized water pipeline regularly in the 29 front water fillings of layering aqueous-phase reflux pump to maintain layering tank median water level.Qualified for guaranteeing tower top acetic acid content, by tower rectifying section sensitive plate and flow tandem, control and realize, simultaneously for water-content in acetic acid at the bottom of assurance tower is qualified, at the bottom of tower, in thick acetic acid, contain a small amount of 2-butyl acetate, the second-class last running of carbon ten, it all sends into acetic acid refining tower 58 and removes the second-class last running of carbon ten under flow control.
On azeotropic tower bottom reboiler 32, pipeline is connected with azeotropy rectification column 35, and bottom line is connected with transferpump at the bottom of tower 31, and at the bottom of tower, transferpump 31 is carried thick acetate products by thick acetic acid line of pipes 30 toward acetic acid refining tower 58.The tower top of azeotropy rectification column 35 is connected with azeotropic overhead condenser 36.
Azeotropic tower bottom reboiler 32 has respectively two pipelines, and one is from pipe network, to carry the steam of 1.5Mpa, and another is the steam condensation water from pipe network, and the material in two pipelines enters azeotropy rectification column 35 after azeotropic tower bottom reboiler 32 mixes.
As shown in Figure 5, the thick ester of azeotropy rectification column 35 tower top outlets first passes through thick ester depickling reactor 44, removes acetic acid, then through 48 separation of ester product tower, obtains ester product.Thick ester depickling reactor 44, is two reactors arranged side by side, in-built special-purpose de-acidying agent, and thick ester, after de-acidying agent bed, removes most acetic acid.In one of them reactor, after special-purpose de-acidying agent inactivation, in the time of can not meeting acetic acid index request, switch and more renew agent.
The blow-down pipe of ester product tower return tank 50 is connected with torch pipe network, the about 30MPa of working pressure, ester product tower reboiler 47 use 1.0MP a steam heating.Tower top steams the lighting ends such as 2-butyl acetate, carbon eight, water, sec-butyl alcohol, through condensing cooling to 40 ℃, enters layering in ester product tower return tank 50, and water is sent azeotropy rectification column return tank 39 back to.Lighting end is returned stream through ester product tower reflux pump 40 parts, and a part is delivered to tank field lighting end storage tank.Under normal running operating mode, side line gas phase extraction 2-butyl acetate product, thick ester first passes through thick ester depickling reactor 44, remove acetic acid, again through 48 separation of ester product tower, obtain ester product, thick ester after depickling enters ester product tower 48 after mixing with one de-salted water under flow control, by the thick ester depickling of pipeline reactor 44, ester product tower 48 and ester product tower condenser 49, ester product reflux tank 50 connects, and in pipeline place installing analysis sampling instrument, ester product tower feed exchanger 46 is arranged on the pipeline of thick ester depickling reactor 44 and ester product tower 48, ester reactor product cooler 45 is connected with ester product tower feed exchanger 46 by pipeline, first after ester product tower feed exchanger 46 and thick ester charging heat exchange, through ester reactor product cooler 45, be cooled to 40 ℃ again, enter ester product surge tank 42, after product introduction ester product surge tank 42, by 2-butyl acetate transferpump 43, deliver to tank field.The second-class last running of carbon ten containing a small amount of 2-butyl acetate concentrating in tower reactor, takes intermittently discharge, delivers to heavies water cooler 56.
When in thick ester raw material, the very low or quality product of last running content is less demanding, not discharging of side line, 2-butyl acetate product by tower at the bottom of extraction, through 2-butyl acetate transferpump 43, send into ester product tower feed exchanger 46, ester reactor product cooler 45, be cooled to after 40 ℃, deliver to tank field.
At the bottom of ester product tower, reboiler 47 has four pipelines, and one is the pipe network from steam, and one is the extremely solidifying grid of steam condensation water, and one is connected with ester product tower 48, and heavies water cooler 56 pipelines connect.
Ester product tower return tank 50 has four pipelines, article one, be the pipeline being connected with ester product tower, article one, be emptying gas to the pipeline of tail gas alkali cleaning of evaporator 66, one be that water is to the pipeline of heavies surge tank 52, this pipeline is installed ester tower return tank water transferpump 41, and the product in ester product tower return tank 50 is delivered to tank field lighting end through ester product through ester product tower reflux pump 40.
As shown in Figure 6, at the bottom of azeotropy rectification column 35 towers, in thick acetic acid, contain the high boiling material such as carbon benzene, and acetic acid has corrodibility, through technological processs such as esterification, decarburization four, azeotropic separation, have microcorrosion; In addition in fresh acetic acid raw material, also contain micro-positively charged ion, for avoiding metallic cation to cause the activity of catalyst for esterification reaction and life-span to reduce, thick acetic acid need to pass through acetic acid refining tower 58, at the bottom of tower, removes high boiling material and metal ion, overhead extraction essence acetic acid, returns to esterification system.Due at the bottom of tower containing the amount of high boiling material seldom, therefore take intermittent mode to control, when concentrate reaches requirement to acetic acid content, then discharge.
The blow-down pipe of acetic acid refining tower return tank 60 is connected with torch pipe network, the about 3KPa of working pressure, and acetic acid refining tower tower bottom reboiler 57 is used 1.5MPa steam heating.Tower top steams acetic acid, through condensing cooling to 45 ℃, by acetic acid refining tower reflux pump 61 parts, is refluxed, and a part is sent acetate buffer tank 5 back to.The high boiling material containing acetic acid (5～15%) concentrating in tower reactor, take intermittently discharge, heavies water cooler 56 is cooled to 40 ℃, through heavies alkali cleaning fresh feed pump 55, get again, entering heavy substance alkali cleaning water cooler 54 mixes with the alkali lye of being got by heavies alkali cleaning recycle pump 53 again, wash, neutralization reaction, enter again heavies alkali cleaning layering tank 62 and carry out the layering of liquid liquid, heavies after separation enters washing heavies surge tank 52, further remove the free liquid of carrying, the heavies after separatory is delivered to tank field storage tank through heavies transferpump 51.
From the heavies at the bottom of ester product tower tower, send into heavies water cooler 56, process equally.When concentration of lye is low to moderate can not meet the demands time, change fresh alkali lye.
Thick acetic acid enters acetic acid refining tower 58 through piping, by pipeline, connect acetic acid refining tower tower bottom reboiler 57, acetic acid refining tower tower bottom reboiler 57 is used 1.5MPa steam heating, tower top steams acetic acid, to acetic acid refining column overhead condenser 59, enter acetic acid refining tower return tank 60, through acetic acid refining tower reflux pump 61, squeeze into acetate buffer tank 5.
Acetic acid refining tower 58 pipelines in top are directly connected with acetic acid refining tower reflux pump 61 transport pipes, and object is that some are transported to acetate buffer tank 5 together containing acetic acid material.
As shown in Figure 7, esterification is thermopositive reaction, for guaranteeing that in reactor, reaction approaches isothermal reaction, takes shell side to pass into circulating hot water heat-obtaining, by controlling hot water temperature and flow, to realize isothermal reaction.
Hot water is extracted out through hot water circulating pump 63 by hot water basin 64, is divided into four tunnels under flow control, sends into respectively in the shell side of esterifier I, II, III, IV, after returning, heat-obtaining reconsolidates Wei Yi road, send into hot water cooler 65, enter hot water basin 64 after cooling, circulate.
As shown in Figure 8, from the emission of each equipment, may contain acetic acid, liquefied gas, ester, nitrogen etc., for guaranteeing that torch pipe network is not corroded, emptying gas need to carry out alkali cleaning.
The emission gases of each equipment is divided two-way supervisor, in one tunnel supervisor, be dropping a hint containing acetate in minute, enter in acetate in minute emptying device 69, another road is the gas that contains dense acetic acid, enters in dense acetic acid emptying device 68, all sends into washing tail gas tank 67, washing tail gas tank 67 bottoms are alkali lye basin, inside establish emptying gas divider, tank top is provided with one section and absorbs washing column, inside establishes 8 blocks of collapsers.During normal running, the acid gas that contains of a small amount of discharge is directly entered by top king-post; When occurring that a large amount of gas is promptly released, portion gas directly enters king-post by top, and a part of gas is in divider enters tank in alkali lye, and part acetic acid is absorbed, and portion gas enters top king-post again.Sodium hydroxide lye in washing tail gas tank 67 is extracted out and is sent into alkali solution cooler 71 absorption column tops through NaOH solution circulating pump 66, the gas containing acetic acid entering with absorption column bottom contacts in collapser, absorb and neutralize, alkali lye returns in V-4302 and circulates again; Gas after the washing of top enters tail gas and divides flow container 70, enters torch pipe network after the alkali lye that separation is carried.After for some time, concentration of lye is low to moderate and can not meets when absorbing neutralization and requiring, and waste water in washing tail gas tank 67 is entered to sewage work, fills into fresh alkali lye.
According to device district landform, sump oil basin 73 can be located at device district below ground, for not allowing sump oil solidify, at sump oil basin 73, hot-water line 74 timing heateds is installed.Live catalyst carries out twice acetic acid immersion conventionally, and it is temporary that the water-containing acetic acid after immersion is put into sump oil basin.After fractionating system goes into operation normally, open sump oil transferpump 72 and water-containing acetic acid is sent into azeotropy rectification column, separating acetic acid and water.The raffinate unification of each equipment enters sump oil basin 73, then sends into azeotropy rectification column Separation and Recovery.
Because decarburization four towers 19, acetic acid refining tower 58 column bottom temperatures are higher, approximately 180 ℃ of left and right, so thermal source need adopt 1.5MPaG steam, and therefore temperature-decreased pressure reducer is installed on each steam gas equipment pipeline.Pressure-controlling table and flow control meter are interconnection.
The present invention can control in real time to whole production technique, product separation is refining and esterification in excessive acetic acid can recycle, economize on resources, can control the temperature of reaction in each reactor, can reduce the corrosion of water-containing acetic acid to equipment, pipeline, the extending catalyst life-span, and can carry out effective alkali cleaning to each equipment tail gas, prevent corrosion and contaminate environment.
Claims (4)
1. 2-butyl acetate production line, is characterized in that: comprise esterification system, separation and purification system and acetic acid recovery system; The exit end of described esterification system is connected with the inlet end of separation and purification system, and the acetic acid exit end of described separation and purification system is connected with the inlet end of acetic acid recovery system, and described acetic acid recovery system is connected with esterification system;
Described esterification system comprises C 4 olefin head tank, coalescer, carbon four strainers, esterifier, acetate buffer tank, acetic acid fresh feed pump, acetic acid cleaner and acetic acid preheater, and described C 4 olefin head tank is connected with mixer entrance with carbon four strainers by coalescer; Described acetate buffer tank is connected with acetic acid cleaner through acetic acid fresh feed pump, and the outlet of acetic acid cleaner is connected with acetic acid preheater inlet end, and described acetic acid preheater is connected with mixer entrance, and described mixer outlet is connected with esterifier;
Described separation and purification system comprises decarburization four devices, azeotropic distillation device, depickling reaction unit and acetic acid refining device; Described decarburization four devices comprise decarburization four towers that are connected with esterifier outlet, described decarburization four towers are connected with decarburization four overhead condensers by decarburization four tower reflux pumps through decarburization four tower return tanks, on decarburization four towers, be also connected with decarburization four tower reboilers and carbon four water wash columns, the top of carbon four water wash columns is connected with washing carbon four surge tanks; Described azeotropic distillation device comprises and the azeotropy rectification column being connected at the bottom of decarburization four tower towers, the tower top of azeotropy rectification column is connected with azeotropic overhead condenser by azeotropy rectification column return tank, the tower top of azeotropy rectification column is connected with carbon four water wash columns, the inlet end of azeotropy rectification column is also connected with fresh acetic acid feed line and greasy dirt transferpump, azeotropy rectification column is provided with transferpump at the bottom of azeotropic tower bottom reboiler and tower, and at the bottom of tower, transferpump is connected with acetic acid refining device by thick acetic acid line of pipes; Described depickling reaction unit comprises thick ester depickling reactor and the ester product tower being connected with azeotropy rectification column by layering ester phase transferpump, ester product tower is connected with ester product condenser, ester product tower bottom reboiler and ester product reflux tank, on the pipeline of thick ester depickling reactor and ester product tower, ester product tower feed exchanger is installed, ester reactor product cooler is connected with ester product tower feed exchanger, ester product tower feed exchanger is connected with ester product surge tank, and ester product tower bottom reboiler is provided with heavies water cooler; Described acetic acid refining device comprises the acetic acid refining tower being connected with azeotropy rectification column, is connected with acetic acid refining tower tower bottom reboiler, acetic acid refining column overhead condenser, acetic acid refining tower return tank and the acetate buffer tank being connected with acetic acid refining tower reflux pump on acetic acid refining tower in turn;
Described acetic acid recovery system comprises and being connected with acetic acid refining tower and the tank connected acetic acid refining tower of acetate buffer reflux pump.
2. 2-butyl acetate production line according to claim 1, is characterized in that: described esterification system also comprises the chain logic device being arranged in esterification pipeline.
3. 2-butyl acetate production line according to claim 1, is characterized in that: described esterifier is shell and tube reactor.
4. 2-butyl acetate production line according to claim 1, is characterized in that: described mixing tank comprises carbon four mixing tanks of two series connection.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892412A (en) * | 2015-06-01 | 2015-09-09 | 石家庄鼎盈化工股份有限公司 | Method for synthesizing benzene-free environment-friendly sec-butyl acetate solvent |
| CN107560321A (en) * | 2017-09-15 | 2018-01-09 | 长江大学 | BOG is reclaimed and nitrogen gas liquefaction system and process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486640A (en) * | 2009-01-13 | 2009-07-22 | 湖南瑞源石化股份有限公司 | Preparation of sec-butyl acetate |
| CN102276452A (en) * | 2011-06-27 | 2011-12-14 | 潍坊亿兴化工科技有限公司 | Production equipment for sec-butyl acetate |
| CN102344353A (en) * | 2010-08-04 | 2012-02-08 | 中国石油化工股份有限公司 | Method for dehydrating acetic acid |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0483826B1 (en) * | 1990-10-31 | 1996-03-13 | Nippon Petrochemicals Company, Limited | Method for producing lower alkyl acetate |
| CN100463897C (en) * | 2007-02-02 | 2009-02-25 | 胡先念 | Method for separating sec-butyl acetate from reaction mixture of acetic acid and hybrid C4 |
| CN202129064U (en) * | 2011-06-27 | 2012-02-01 | 潍坊亿兴化工科技有限公司 | Sec-butyl acetate reaction unit |
| CN202688237U (en) * | 2012-04-20 | 2013-01-23 | 临沂市金沂蒙生物科技有限公司 | Production device for n-butyl acetate |
| CN102964244B (en) * | 2012-11-16 | 2017-04-05 | 北京石油化工学院 | The separation method of refined sec-Butyl Acetate |
-
2014
- 2014-06-23 CN CN201410279570.9A patent/CN104109088B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486640A (en) * | 2009-01-13 | 2009-07-22 | 湖南瑞源石化股份有限公司 | Preparation of sec-butyl acetate |
| CN102344353A (en) * | 2010-08-04 | 2012-02-08 | 中国石油化工股份有限公司 | Method for dehydrating acetic acid |
| CN102276452A (en) * | 2011-06-27 | 2011-12-14 | 潍坊亿兴化工科技有限公司 | Production equipment for sec-butyl acetate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892412A (en) * | 2015-06-01 | 2015-09-09 | 石家庄鼎盈化工股份有限公司 | Method for synthesizing benzene-free environment-friendly sec-butyl acetate solvent |
| CN104892412B (en) * | 2015-06-01 | 2016-08-24 | 石家庄鼎盈化工股份有限公司 | A kind of synthetic method of the secondary butyl ester of benzene-free and environment-friendly solvent acetic acid |
| CN107560321A (en) * | 2017-09-15 | 2018-01-09 | 长江大学 | BOG is reclaimed and nitrogen gas liquefaction system and process |
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