CN102675090B - Deep oxidation method in polymerization-grade Production of Terephthalic Acid and deep oxidation device - Google Patents
Deep oxidation method in polymerization-grade Production of Terephthalic Acid and deep oxidation device Download PDFInfo
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Abstract
The present invention relates to the deep oxidation method in a kind of KPTA production and deep oxidation device, described method comprises the steps: that (1) is oxidized, and uses dioxygen oxidation PX under catalytic condition in solvent HAC; (2) deep oxidation, is oxidized the further deep oxidation of slurry oxygen that obtains to improve TA content by step (1); (3) crystallization, separation, crystallization from the slurry that step (2) obtains, separation TA.Described system comprises oxidation reactor, reactor discharge tank, deep oxidization reactor and Crystallization Separation system, the slurry outlet of described oxidation reactor connects the slurry import of discharge tank, the slurry outlet of described discharge tank connects the slurry import of deep oxidization reactor, and the slurry outlet of described deep oxidization reactor connects the slurry import of described Crystallization Separation system.Method of the present invention can ensure quality product, also reduces the requirement to equipment, and its system eliminates whipping device, reduces facility investment, and effectively reduces power consumption.
Description
Technical field
The present invention relates to KPTA(the Kunlun company polymerization-grade terephthalic acid) produce in deep oxidation method, also relate to a kind of deep oxidation device adopting the method, belong to chemical technology field.
Background technology
The Technology of producing terephthalic acid at present in the world has two kinds: one is PTA(pure terephthalic acid) production technique, device is divided into oxidation unit and hydrofining unit two parts.Under catalyst action, first p-Xylol (PX) is generated in acetic acid (HAC) solvent terephthalic acid (TA) and intermediate product (p-carboxybenzaldehyde 4-CBA, p-methylbenzoic acid PT acid etc.) with dioxygen oxidation in air, produce crude terephthalic acid (CTA), then CTA is soluble in water, 4-CBA is made to be reduced into PT acid by hydrogenation reaction, utilize PT acid and TA different solubility in water, make PT acid be separated with TA after filtration, generate pure PTA.This technique major defect is that flow process is longer, investment and energy consumption relatively high.
Another kind of production line is deep oxidation method, after namely PX generates TA and intermediate product with dioxygen oxidation in air in HAC solvent, continues to pass into air and makes its deep oxidation, and PT acid and 4-CBA generate TA further.Deep oxidization technique has the advantage that flow process is short, reduced investment, sewage are few, but conventional depth oxidizing reaction technique adopts whipping device many, and Energy harvesting is unreasonable, and impurity removed system is complicated, and recent two decades, without too many development, does not set up new factory yet.Current employing deep oxidization technique produces the manufacturer of TA, and oxidation and deep oxidization reactor mostly adopt stirred-tank reactor, invest high, consume a large amount of electric energy.
Summary of the invention
In order to overcome the above-mentioned defect of prior art, a kind of deep oxidation method in the object of the present invention is to provide KPTA to produce and deep oxidation device, with simplified apparatus structure, reduce energy expenditure, handled easily, reduce construction investment and running cost.
The present invention realizes the technical scheme that above-mentioned purpose adopts:
A deep oxidation method during KPTA produces, comprises the steps:
(1) rear oxidation is oxidized:
The slurry that oxidation reactor is discharged is sent into described discharge tank from the middle part of discharge tank, oxygen-containing gas (such as pressurized air and deep oxidation tail gas) is sent into described discharge tank from the bottom of described discharge tank, described oxygen-containing gas is made to mix slurry from the bottom bubbling of described discharge tank, to impel the suspended solid in described slurry not precipitate under the mixing of oxygen-containing gas, described slurry comprises PT acid and 4-CBA proceeds rear oxidation at interior intermediate oxidation product and reacts in described discharge tank with oxygen;
(2) deep oxidation:
The bottom slurry of described discharge tank is discharged from the slurry outlet bottom described discharge tank, deep oxidization reactor is sent into after Pressurized-heated, oxygen-containing gas is sent into described deep oxidization reactor from the bottom of described deep oxidization reactor, described oxygen-containing gas is made to mix slurry from the bottom bubbling of described deep oxidization reactor, do not precipitate under the mixing of oxygen-containing gas to impel the suspended solid in described slurry, described slurry comprises PT acid and 4-CBA proceeds with oxygen to be oxidized at interior intermediate oxidation product in described deep oxidization reactor, described deep oxidization reactor discharges deep oxidation tail gas under pressure-controlling, discharge under Liquid level deep oxidation reacted after slurry.
Preferably, to be discharged by described oxidation reactor and the PT acid content sent in the slurry of described discharge tank is 8500-9500ppm, 4-CBA content is 3500-4500ppm, to be discharged by described discharge tank and the PT acid content sending into the slurry of described deep oxidization reactor is 450-550ppm, 4-CBA content is 2000-3000ppm, PT acid content in slurry after described deep oxidation has reacted is 20-50ppm, 4-CBA content is 100-180ppm.
Preferably, the oxygen-containing gas of the described deep oxidization reactor of described feeding is fresh air and the mixed pressurization gas of oxidizing reaction tail gas after purifying, control the oxygen level of described pressurization gas in certain scope, the pressure of described pressurization gas is 4.5-4.8MPaG, the reaction conditions of described deep oxidation is: temperature 220 DEG C ~ 250 DEG C, pressure 1.5MPaG ~ 4.6MPaG.
Preferably, the oxygen-containing gas of the described discharge tank of described feeding comprises fresh air and deep oxidation tail gas, the slurry import of described discharge tank is positioned at the middle part of described discharge tank, and be communicated with the slurry outlet be positioned at bottom described oxidation reactor by pipeline, to realize slurry by the conveying of described oxidation reactor to described discharge tank, the top tail gas of described discharge tank enters described oxidation reactor by pipeline, described discharge tank is provided with by the control valve of the Liquid level of described oxidation reactor to the pipeline of described deep oxidization reactor conveying slurry, according to the Liquid level of described oxidation reactor, the slurry of discharge tank is discharged.
Preferably, described deep oxidization reactor is made up of the deep oxidization reactor I connected successively and deep oxidization reactor II, the slurry that described discharge tank is discharged sends into described deep oxidization reactor I from the slurry import be positioned in the middle part of described deep oxidization reactor I, described pressurization gas sends into described deep oxidization reactor I from the bottom of described deep oxidization reactor I, slurry outlet bottom described deep oxidization reactor I sends into the slurry import in the middle part of described deep oxidization reactor II by deep oxidation slurry vent pipe I, described deep oxidation slurry vent pipe I is provided with by the control valve of the Liquid level of described deep oxidization reactor I, according to the Liquid level of described deep oxidization reactor I, the slurry of deep oxidization reactor I is discharged, the top tail gas of described deep oxidization reactor I sends into described deep oxidization reactor II by deep oxidation exhaust emission tube I from the bottom of described deep oxidization reactor II, mix slurry at the bottom bubbling of described deep oxidization reactor II and form the oxygen sources of described deep oxidization reactor II, described deep oxidation exhaust emission tube I is provided with by the pressure controlled control valve of described deep oxidization reactor I, according to the pressure-controlling in described deep oxidization reactor I, the tail gas of deep oxidization reactor I is discharged, slurry outlet bottom described deep oxidization reactor II connects deep oxidation slurry vent pipe II, described deep oxidation slurry vent pipe II is provided with by the control valve of the Liquid level of described deep oxidization reactor II, according to the Liquid level of described deep oxidization reactor II, the slurry of deep oxidization reactor II is discharged, the deep oxidation tail gas at described deep oxidization reactor II top is discharged by deep oxidation exhaust emission tube II and accesses the exothermic medium import of deep oxidation exhaust gas heat exchanger, heat exchange is carried out with the steam condensate being used as heat-absorbing medium in described deep oxidation exhaust gas heat exchanger, described steam condensate is absorbed heat and becomes byproduct steam, the exothermic medium outlet of described deep oxidation exhaust gas heat exchanger connects the deep oxidation exhaust pipe being used for sending into described deep oxidation tail gas to described discharge tank, described deep oxidation exhaust pipe is provided with the pressure controlled control valve by described deep oxidization reactor II, the discharge of deep oxidation tail gas according to the pressure-controlling of described deep oxidization reactor II.
Preferably, according to end product quality change regulation depth degree of oxidation, comprise the temperature of reaction in the described deep oxidization reactor of adjustment and the residence time of slurry in described deep oxidization reactor, the adjustment of described deep oxidation temperature is realized by the pressure size controlled in described deep oxidization reactor, and the adjustment of the described residence time is realized by the height of liquid level controlling described deep oxidization reactor.
Preferably, the service temperature of described deep oxidization reactor I is 230 DEG C ~ 250 DEG C, pressure is 4.5MPaG ~ 4.6MPaG, the service temperature of described deep oxidization reactor II is 220 DEG C ~ 230 DEG C, pressure is 1.5MPaG ~ 2.0MPaG, and the pressure of described deep oxidization reactor II is lower than the pressure of described deep oxidization reactor I.
A kind of deep oxidation device adopted in the KPTA production of above-mentioned each method, it comprises the discharge tank and deep oxidization reactor that connect successively, described deep oxidization reactor is single deep oxidization reactor, or be made up of the deep oxidization reactor I connected successively and deep oxidization reactor II, described discharge tank, deep oxidization reactor I and deep oxidization reactor II all adopts bubble tower, bottom is equipped with inlet mouth, described inlet mouth connects oxygen-containing gas pipeline, described oxygen-containing gas enters described discharge tank from corresponding described inlet mouth, after deep oxidization reactor I or deep oxidization reactor II, at described discharge tank, the bottom bubbling of deep oxidization reactor I or deep oxidization reactor II mixes slurry, do not precipitate under the mixing of oxygen-containing gas to impel the suspended solid in described slurry, described discharge tank, slurry in deep oxidization reactor I or deep oxidization reactor II comprises PT acid and 4-CBA proceeds oxidizing reaction at interior intermediate oxidation product and oxygen.
Preferably, the length-to-diameter ratio of described discharge tank is 6 ~ 10, volume is no more than 15% of oxidation reactor supporting in described deep oxidation method KPTA production, the length-to-diameter ratio of described deep oxidization reactor I and described deep oxidization reactor II is 5 ~ 8, and the volume sum of the two is no more than 80% of described oxidation reactor.
Preferably, the slurry import of described discharge tank is positioned at the middle part of described discharge tank, and be communicated with the slurry outlet bottom described oxidation reactor by pipeline, to realize slurry by the conveying of described oxidation reactor to described discharge tank, the top of described discharge tank is provided with tail gas relief outlet, and the liquid phase region of described oxidation reactor is connected by discharge tank exhaust pipe, with inverted U-shaped on described discharge tank exhaust pipe, described discharge tank carries the pipeline of slurry to be provided with by the control valve of the Liquid level of described oxidation reactor to described deep oxidization reactor I, according to the Liquid level of described oxidation reactor, the slurry of discharge tank is discharged, described discharge tank is carried on the pipeline of slurry to described deep oxidization reactor I and is also connected with paste heater, described paste heater is provided with steam pipeline (trace), the heating of described slurry is given by steam, described steam pipeline (trace) is provided with the temperature controlled control valve by described deep oxidization reactor I, the heating of described paste heater is controlled according to the temperature of described deep oxidization reactor I, inlet mouth bottom described discharge tank comprises compressed air inlet and deep oxidation inlet exhaust gas, described compressed air inlet connects compressed air line or air compressor machine, described deep oxidation inlet exhaust gas connects the deep oxidation tail gas relief outlet at described deep oxidization reactor II top by deep oxidation exhaust pipe, described deep oxidation exhaust pipe is provided with the control valve by the pressure of described deep oxidization reactor II, the discharge of deep oxidation tail gas according to the pressure-controlling in described deep oxidization reactor II, deep oxidation exhaust gas heat exchanger is provided with between the deep oxidation tail gas relief outlet at described deep oxidation exhaust pipe and described deep oxidization reactor II top, described deep oxidation exhaust pipe connects the exothermic medium outlet of described deep oxidation exhaust gas heat exchanger, the deep oxidation tail gas relief outlet at described deep oxidization reactor II top connects the exothermic medium import of described deep oxidation exhaust gas heat exchanger, the heat-absorbing medium import of described deep oxidation exhaust gas heat exchanger connects steam condensate pipe, described steam condensate forms byproduct steam after the heat exchange of described deep oxidation exhaust gas heat exchanger.
Preferably, the inlet mouth of described deep oxidization reactor I connects pressurization gas pipeline, described pressurization gas pipeline is connected with the compressor for gas boosting, the inlet mouth of described compressor connects compressed air line and the oxidation reactor exhaust pipe after purifying, slurry outlet bottom described deep oxidization reactor I sends into the slurry import in the middle part of described deep oxidization reactor II by deep oxidation slurry vent pipe I, described deep oxidation slurry vent pipe I is provided with by the control valve of the Liquid level of described deep oxidization reactor I, according to the Liquid level of described deep oxidization reactor I, the slurry of deep oxidization reactor I is discharged, the top offgas outlet of described deep oxidization reactor I connects the inlet mouth bottom described deep oxidization reactor II by deep oxidation exhaust emission tube I, described deep oxidation exhaust emission tube I is provided with by the pressure controlled control valve of described deep oxidization reactor I, according to the pressure-controlling in described deep oxidization reactor I, the tail gas of deep oxidization reactor I is discharged, slurry outlet bottom described deep oxidization reactor II connects deep oxidation slurry vent pipe II, described deep oxidation slurry vent pipe II is provided with by the control valve of the Liquid level of described deep oxidization reactor II, according to the Liquid level of described deep oxidization reactor II, the slurry of deep oxidization reactor II is discharged.
The invention has the beneficial effects as follows:
The present invention adopts medium temperature and medium pressure deep oxidation to significantly reduce the content of the intermediate product 4-CBA in KPTA, and bubbling column reactor is while eliminating whipping device, also effectively prevent the precipitation of suspended nitride, in addition for mix with the air in dispersion phase for, also improve the Gas content in reaction liquid phase, be conducive to the efficiency improving oxidizing reaction, not only reduce the facility investment of about 50%, also save stirring power consumption, for the system of megaton, facility investment 4,000 ten thousand yuan can be reduced, reduce power consumption 1000kwh/h.
The present invention is also provided with oxidation rear oxidation between oxidizing reaction and deep oxidation reaction, not only be conducive to anti-oxidation discharging to be short-circuited, but also improve oxidation effectiveness, be conducive to alleviating follow-up deep oxidation reaction requirement, according to the intermediate product characteristic in slurry, the reaction conditions of oxidation rear oxidation can also be reasonably set simultaneously, and by the Collaborative Control with oxidation reactor, while handled easily, make W-response flow process and reaction conditions more reasonable.
The tail gas of each reactor can be back to native system, reduce further energy consumption, decreases the discharge of tail gas and decreases the treatment capacity of tail gas, achieving many things at one stroke.
Processing parameter of the present invention arranges rationally, and regulation and control is simply effective, meets slurry in the reaction characteristics of different steps and cooperatively interacting of each stage, is conducive to the steady running of keeping system, improves productive rate.
Accompanying drawing explanation
Fig. 1 is the main chemical reactions schematic diagram that the present invention relates to;
Fig. 2 is the one-piece construction schematic diagram of an embodiment of system of the present invention;
Fig. 3 is the one-piece construction schematic diagram of another embodiment of system of the present invention.
Embodiment
See Fig. 1-3, in deep oxidation device provided by the invention, all adopting the tower reactor without stirring, saving stirring electricity consumption, simplifying equipment, investment also significantly reduces.
The present invention relates to be oxidized by PX and generate the process of TA, go through many middle chemical reactions, its principal reaction process is as shown in Figure 1, and the activation energy of each intermediate reaction is as follows:
K1---PX oxidation generates TALD(p-tolyl aldehyde), activation energy 65kJ/mol
K2---TALD oxidation generates PT acid (p-methylbenzoic acid), activation energy 51.5kJ/mol
K3---PT acid oxidase generates 4-CBA(p-carboxybenzaldehyde), activation energy 85.1kJ/mol
K4---4-CBA oxidation generates TA(terephthalic acid), activation energy 78.3kJ/mol
From reaction complexity, the soonest, it is the slowest that the 3rd step PT acid generates 4-CBA reaction to first and second step speed of response, and it is also relatively easy that the 4th step 4-CBA reacts generation TA further.So oxidizing reaction discharges contained PT acid maximum (~ 9000ppm) in slurry, because PT acid is soluble in HAC, so PT acid is mostly present in the liquid phase in slurry.Although 4-CBA content only has ~ 4000ppm in reaction paste, due to cocrystallization reason, 4-CBA is present in solid phase mostly.Deep oxidation reaction is exactly make PT acid oxidase generate 4-CBA, 4-CBA to be oxidized generation TA further again.Obviously, because 4-CBA major part is present in solid phase, want further oxidation, 4-CBA first will be made to diffuse out from crystalline solid phase, so deep oxidation reaction will at high temperature make the TA in slurry all dissolve or be partly dissolved, could be oxidized after 4-CBA enters liquid phase and generate TA.
Deep oxidation reaction is not fierce, requires not high to mass-and heat-transfer yet, the reactor that conventional depth oxidizing reaction adopts band to stir, and object avoids suspended nitride to deposit, and mix dispersion air, increases reactor gas holdup.
In the embodiment shown in Figure 2, PX, circulation HAC and catalyst by proportion send into the oxidation reactor of bubble tower type, reactor bottom passes into technique pressurized air, oxidizing reaction is carried out under temperature 186 ~ 188 DEG C, pressure ~ 1.25MpaA condition, generate TA and intermediate product, reaction paste exports and enters discharge tank bottom oxidation reactor, discharge tank bottom passes into deep oxidation tail gas and fresh air, bubbling mixes slurry, solid suspension is not deposited, and makes intermediate oxidation product (PT acid, 4-CBA etc.) continue oxidation.Discharge tank top tail gas enters oxidation reactor, bottom discharge tank, slurry is (containing PT acid ~ 500ppm, 4-CBA ~ 2500ppm), after mashing pump boosting and heater heats, penetration depth oxidation reactor middle and upper part, tail gas and the mixing of some processes pressurized air after treatment and purification, through supercharging (~ 4.8MpaG, such as 4.5-4.8MPaG) send into bubbling bottom deep oxidization reactor afterwards and mix slurry, deep oxidation reaction is temperature 220 ~ 250 DEG C, carry out under pressure 1.5 ~ 4.6MPaG condition, make PT acid, 4-CBA be oxidized further generate TA.Deep oxidation tail gas is discharged in deep oxidization reactor top under pressure-controlling, and this tail gas is mixed gas as oxidizing reaction discharge tank and used, slurry (PT acid content ~ 50ppm, such as 20-50ppm that deep oxidation has reacted; 4-CBA ~ 150ppm, such as 100-180ppm), under Liquid level, enter crystal system.
The effect of described discharge tank, one is that anti-oxidation discharging is short-circuited, and two is rear oxidations.Do not deposit to ensure gas holdup that in discharge tank, material is enough and fully mixing slurry, discharge tank design length-to-diameter ratio 6 ~ 10, the suitable oxidation reactor 10 ~ 15% of volume, deep oxidation tail gas and/or pressurized air input and output material bottom of the barrel can arrange suitable air intake structure, to form better bubbling effect, deep oxidation tail gas and pressurized air can enter discharge tank respectively, also can enter discharge tank together with the form of mixed gas or be mixed in intake process by the same import of access.
Deep oxidization reactor opening for feed is located at middle and upper part, and bottom air inlet adopts special construction, reaches and mixes suspended nitride effect.Deep oxidization reactor design length-to-diameter ratio is 5 ~ 8, and volume is approximately 70 ~ 80% of oxidation reactor, by Liquid level regulation depth oxidization time.
As shown in Figure 3, deep oxidization reactor is preferably designed to the reactor of two series connection, second deep oxidization reactor (deep oxidization reactor II) control pressure will lower than the first deep oxidization reactor (deep oxidization reactor I), so that discharge and step-down, how to select to select by requirement of engineering.
Enter the oxidizing reaction slurry of discharge tank, make it mix suspension with deep oxidation tail gas, and continue oxidation, make a large amount of PT acid generate 4-CBA, part 4-CBA generates TA further.The tail gas that discharge tank top is collected, enters oxidizing reaction liquid phase by " ∩ " type (inverted U-shaped) curved pipe, finally enters oxidized tail gas system.Discharge tank bottom slurry topping-up pump is extracted out, with the sendout of Liquid level topping-up pump.Before slurry penetration depth oxidation reactor I, by 60 ~ 80bar steam heating, its degree of heat is controlled by deep oxidation temperature of reaction.Pass into the pressurization gas mixed by tail gas after purifying and pressurized air in deep oxidization reactor I bottom, make slurry suspension in reactor, and make PT acid and 4-CBA oxidation generation TA in liquid phase.Deep oxidization reactor I service temperature 230 ~ 250 DEG C, pressure 4.0 ~ 4.6MPaG, preferred 4.5MPaG ~ 4.6MPaG.
Deep oxidization reactor I slurry enters deep oxidization reactor II middle and upper part under Liquid level, deep oxidization reactor I top tail gas passes into bottom deep oxidization reactor II under pressure-controlling, deep oxidization reactor II service temperature 220 ~ 230 DEG C, pressure 1.5 ~ 2.0MPaG.Deep oxidization reactor II regulates temperature of reaction with pressure.The effect of deep oxidization reactor II is:
(1) reaction has been tended to
(2) product cut size is regulated
Slurry after deep oxidation enters crystal system under Liquid level.
According to end product quality change regulation depth degree of oxidation, its control device is percentage regulation oxidizing temperature and the residence time, the adjustment of deep oxidation temperature realizes by pressure-controlling, and the control of reaction time has come by regulation depth oxidation reactor height of liquid level.
KPTA deep oxidization technique of the present invention is medium temperature and medium pressure technology, the device structure not only adopted differs from other manufacturers in the world, in the control of processing parameter, be both different from the deep oxidization technique of high temperature, high pressure TA solid CL, also differed greatly with low-temp low-pressure diffusion deep oxidation method.
The present invention is by changing the structure of each reactor, mechanical stirring is substituted with gas sparging, and change the condition of deep oxidation reaction, medium temperature and medium pressure is changed into by the high-temperature and high-pressure conditions under prior art, reduce material requirements and the processing requirement of equipment, not only invest decline (fall about 50%) thus, and save agitator power consumption.Concerning megaton PTA device, compared with traditional technology, can reduce investment outlay ~ 4,000 ten thousand yuan, electric consumption can save ~ 1000kWh/h.
Claims (3)
1. the deep oxidation method in polymerization-grade Production of Terephthalic Acid, comprises the steps:
(1) rear oxidation is oxidized:
The slurry that oxidation reactor is discharged is sent into described discharge tank from the middle part of discharge tank, the bottom of oxygen-containing gas from described discharge tank is entered, described oxygen-containing gas is made to mix slurry from the bottom bubbling of described discharge tank, do not precipitate under the mixing of oxygen-containing gas to impel the suspended solid in described slurry, described slurry comprises PT acid and 4-CBA proceeds rear oxidation at interior intermediate oxidation product and reacts in described discharge tank with oxygen, and the described oxygen-containing gas sending into described discharge tank comprises fresh air and deep oxidation tail gas;
(2) deep oxidation:
The bottom slurry of described discharge tank is discharged from the slurry outlet bottom described discharge tank, deep oxidization reactor is sent into after Pressurized-heated, oxygen-containing gas is sent into described deep oxidization reactor from the bottom of described deep oxidization reactor, described oxygen-containing gas is made to mix slurry from the bottom bubbling of described deep oxidization reactor, do not precipitate under the mixing of oxygen-containing gas to impel the suspended solid in described slurry, described slurry comprises PT acid and 4-CBA proceeds with oxygen to be oxidized at interior intermediate oxidation product in described deep oxidization reactor, described deep oxidization reactor discharges deep oxidation tail gas under pressure-controlling, slurry after deep oxidation has reacted enters crystal system under Liquid level, the described oxygen-containing gas sending into described deep oxidization reactor is fresh air and the mixed pressurization gas of oxidizing reaction tail gas after purifying,
To be discharged by described oxidation reactor and the PT acid content sent in the slurry of described discharge tank is 8500-9500ppm, 4-CBA content is 3500-4500ppm, to be discharged by described discharge tank and the PT acid content sending into the slurry of described deep oxidization reactor is 450-550ppm, 4-CBA content is 2000-3000ppm, PT acid content in slurry after described deep oxidation has reacted is 20-50ppm, 4-CBA content is 100-180ppm
Described discharge tank design length-to-diameter ratio 6 ~ 10, the suitable oxidation reactor 10 ~ 15% of volume, the slurry import of described discharge tank is positioned at the middle part of described discharge tank, and be communicated with the slurry outlet be positioned at bottom described oxidation reactor by pipeline, to realize slurry by the conveying of described oxidation reactor to described discharge tank, the tail gas that described discharge tank top is collected enters oxidizing reaction liquid phase by inverted U-shaped curved pipe, described discharge tank is provided with by the control valve of the Liquid level of described oxidation reactor to the pipeline of described deep oxidization reactor conveying slurry, according to the Liquid level of described oxidation reactor, the slurry of discharge tank is discharged,
Described deep oxidization reactor is made up of the deep oxidization reactor I connected successively and deep oxidization reactor II, the slurry that described discharge tank is discharged sends into described deep oxidization reactor I from the slurry import be positioned in the middle part of described deep oxidization reactor I, described pressurization gas sends into described deep oxidization reactor I from the bottom of described deep oxidization reactor I, slurry outlet bottom described deep oxidization reactor I sends into the slurry import in the middle part of described deep oxidization reactor II by deep oxidation slurry vent pipe I, described deep oxidation slurry vent pipe I is provided with by the control valve of the Liquid level of described deep oxidization reactor I, according to the Liquid level of described deep oxidization reactor I, the slurry of deep oxidization reactor I is discharged, the top tail gas of described deep oxidization reactor I sends into described deep oxidization reactor II by deep oxidation exhaust emission tube I from the bottom of described deep oxidization reactor II, mix slurry at the bottom bubbling of described deep oxidization reactor II and form the oxygen sources of described deep oxidization reactor II, described deep oxidation exhaust emission tube I is provided with by the pressure controlled control valve of described deep oxidization reactor I, according to the pressure-controlling in described deep oxidization reactor I, the tail gas of deep oxidization reactor I is discharged, slurry outlet bottom described deep oxidization reactor II connects deep oxidation slurry vent pipe II, described deep oxidation slurry vent pipe II is provided with by the control valve of the Liquid level of described deep oxidization reactor II, according to the Liquid level of described deep oxidization reactor II, the slurry of deep oxidization reactor II is discharged, the deep oxidation tail gas at described deep oxidization reactor II top is discharged by deep oxidation exhaust emission tube II and accesses the exothermic medium import of deep oxidation exhaust gas heat exchanger, heat exchange is carried out with the steam condensate being used as heat-absorbing medium in described deep oxidation exhaust gas heat exchanger, described steam condensate is absorbed heat and becomes byproduct steam, the exothermic medium outlet of described deep oxidation exhaust gas heat exchanger connects the deep oxidation exhaust pipe being used for sending into described deep oxidation tail gas to described discharge tank, described deep oxidation exhaust pipe is provided with the pressure controlled control valve by described deep oxidization reactor II, the discharge of deep oxidation tail gas according to the pressure-controlling of described deep oxidization reactor II
According to end product quality change regulation depth degree of oxidation, comprise the temperature of reaction in the described deep oxidization reactor of adjustment and the residence time of slurry in described deep oxidization reactor, the adjustment of described deep oxidation temperature is realized by the pressure size controlled in described deep oxidization reactor, the adjustment of the described residence time is realized by the height of liquid level controlling described deep oxidization reactor, the service temperature of described deep oxidization reactor I is 230 DEG C ~ 250 DEG C, pressure is 4.5MPaG ~ 4.6MPaG, the service temperature of described deep oxidization reactor II is 220 DEG C ~ 230 DEG C, pressure is 1.5MPaG ~ 2.0MPaG, the pressure of described deep oxidization reactor II is lower than the pressure of described deep oxidization reactor I.
2. the deep oxidation device in a polymerization-grade Production of Terephthalic Acid, it is characterized in that comprising the discharge tank and deep oxidization reactor that connect successively, described discharge tank design length-to-diameter ratio 6 ~ 10, the suitable oxidation reactor 10 ~ 15% of volume, the slurry import of described discharge tank is positioned at the middle part of described discharge tank, and be communicated with the slurry outlet be positioned at bottom described oxidation reactor by pipeline, to realize slurry by the conveying of described oxidation reactor to described discharge tank, the top tail gas of described discharge tank enters described oxidation reactor by pipeline, described discharge tank is provided with by the control valve of the Liquid level of described oxidation reactor to the pipeline of described deep oxidization reactor conveying slurry, according to the Liquid level of described oxidation reactor, the slurry of discharge tank is discharged, described deep oxidization reactor is made up of the deep oxidization reactor I connected successively and deep oxidization reactor II, described discharge tank, deep oxidization reactor I and deep oxidization reactor II all adopts bubble tower, bottom is equipped with inlet mouth, described inlet mouth connects oxygen-containing gas pipeline, described oxygen-containing gas enters described discharge tank from corresponding described inlet mouth, after deep oxidization reactor I or deep oxidization reactor II, at described discharge tank, the bottom bubbling of deep oxidization reactor I or deep oxidization reactor II mixes slurry, do not precipitate under the mixing of oxygen-containing gas to impel the suspended solid in described slurry, described discharge tank, slurry in deep oxidization reactor I or deep oxidization reactor II comprises PT acid and 4-CBA proceeds oxidizing reaction at interior intermediate oxidation product and oxygen, the inlet mouth of described deep oxidization reactor I connects pressurization gas pipeline, described pressurization gas pipeline is connected with the compressor for gas boosting, the inlet mouth of described compressor connects compressed air line and the oxidation reactor exhaust pipe after purifying, compressed air inlet and deep oxidation inlet exhaust gas is provided with bottom described discharge tank, described compressed air inlet connects compressed air line or air compressor machine, described deep oxidation inlet exhaust gas connects the deep oxidation tail gas relief outlet at described deep oxidization reactor II top by deep oxidation exhaust pipe,
The length-to-diameter ratio of described deep oxidization reactor I and described deep oxidization reactor II is 5 ~ 8, and the volume sum of the two is no more than 70 ~ 80% of described oxidation reactor,
The slurry import of described discharge tank is positioned at the middle part of described discharge tank, and be communicated with the slurry outlet bottom described oxidation reactor by pipeline, to realize slurry by the conveying of described oxidation reactor to described discharge tank, the top that the top tail gas of described discharge tank is described discharge tank by the mode that pipeline enters described oxidation reactor is provided with tail gas relief outlet, and the liquid phase region of described oxidation reactor is connected by discharge tank exhaust pipe, with inverted U-shaped on described discharge tank exhaust pipe, described discharge tank is carried on the pipeline of slurry to described deep oxidization reactor I and is also connected with paste heater, described paste heater is provided with steam pipeline (trace), the heating of described slurry is given by steam, described steam pipeline (trace) is provided with the temperature controlled control valve by described deep oxidization reactor I, the heating of described paste heater is controlled according to the temperature of described deep oxidization reactor I, described deep oxidation exhaust pipe is provided with the pressure controlled control valve by described deep oxidization reactor II, the discharge of deep oxidation tail gas according to the pressure-controlling in described deep oxidization reactor II, deep oxidation exhaust gas heat exchanger is provided with between the deep oxidation tail gas relief outlet at described deep oxidation exhaust pipe and described deep oxidization reactor II top, described deep oxidation exhaust pipe connects the exothermic medium outlet of described deep oxidation exhaust gas heat exchanger, the deep oxidation tail gas relief outlet at described deep oxidization reactor II top connects the exothermic medium import of described deep oxidation exhaust gas heat exchanger, the heat-absorbing medium import of described deep oxidation exhaust gas heat exchanger connects steam condensate pipe, described steam condensate forms byproduct steam after the heat exchange of described deep oxidation exhaust gas heat exchanger.
3. device as claimed in claim 2, it is characterized in that slurry outlet bottom described deep oxidization reactor I sends into the slurry import in the middle part of described deep oxidization reactor II by deep oxidation slurry vent pipe I, described deep oxidation slurry vent pipe I is provided with by the control valve of the Liquid level of described deep oxidization reactor I, according to the Liquid level of described deep oxidization reactor I, the slurry of deep oxidization reactor I is discharged, the top offgas outlet of described deep oxidization reactor I connects the bottom air inlet of described deep oxidization reactor II by deep oxidation exhaust emission tube I, described deep oxidation exhaust emission tube I is provided with by the pressure controlled control valve of described deep oxidization reactor I, according to the pressure-controlling in described deep oxidization reactor I, the tail gas of deep oxidization reactor I is discharged, slurry outlet bottom described deep oxidization reactor II connects deep oxidation slurry vent pipe II, described deep oxidation slurry vent pipe II is provided with by the control valve of the Liquid level of described deep oxidization reactor II, according to the Liquid level of described deep oxidization reactor II, the slurry of deep oxidization reactor II is discharged.
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| CN109251139B (en) * | 2018-11-02 | 2021-06-25 | 中国石油天然气集团有限公司 | PIA production method and production system adopting deep oxidation |
| CN111569454B (en) * | 2020-03-31 | 2021-07-09 | 南京延长反应技术研究院有限公司 | Built-in micro-interface oxidation system and method for preparing terephthalic acid from p-xylene |
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| US4772748A (en) * | 1982-12-10 | 1988-09-20 | Mitsubishi Chemical Industries Limited | Process for producing highly pure terephthalic acid |
| CN2910344Y (en) * | 2005-11-18 | 2007-06-13 | 浙江大学 | Bubbling tower oxidizing apparatus for production of aromatic carboxyl acid |
| CN201704239U (en) * | 2010-04-30 | 2011-01-12 | 中国石油天然气集团公司 | Paraxylene oxidation crystallization device |
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| CN2654608Y (en) * | 2003-10-12 | 2004-11-10 | 浙江大学 | Bubbling tower oxidation reaction device for producing terephthalic acid |
| CN202700501U (en) * | 2012-05-15 | 2013-01-30 | 中国昆仑工程公司 | Stirring-free oxidating and deep-oxidating reaction system applicable to KPTA (Kunlun pure terephthalic acid) production |
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| US4772748A (en) * | 1982-12-10 | 1988-09-20 | Mitsubishi Chemical Industries Limited | Process for producing highly pure terephthalic acid |
| CN2910344Y (en) * | 2005-11-18 | 2007-06-13 | 浙江大学 | Bubbling tower oxidizing apparatus for production of aromatic carboxyl acid |
| CN201704239U (en) * | 2010-04-30 | 2011-01-12 | 中国石油天然气集团公司 | Paraxylene oxidation crystallization device |
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