CN101537299B - Method for recycling organic matters in tail gas from production of terephthalic acid - Google Patents
Method for recycling organic matters in tail gas from production of terephthalic acid Download PDFInfo
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- CN101537299B CN101537299B CN2009100967911A CN200910096791A CN101537299B CN 101537299 B CN101537299 B CN 101537299B CN 2009100967911 A CN2009100967911 A CN 2009100967911A CN 200910096791 A CN200910096791 A CN 200910096791A CN 101537299 B CN101537299 B CN 101537299B
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- methyl acetate
- tail gas
- acetic acid
- purifying column
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Abstract
The invention discloses a method for recycling organic matters in tail gas from production of terephthalic acid, the tail gas from the production of terephthalic acid is introduced into a high-pressure absorption tower for absorbing para-xylene, methyl acetate and acetic acid in the tail gas; absorption liquid at the bottom part of the high-pressure absorption tower is sent to a methyl acetate purifying tower, distillate at the top of the methyl acetate purifying tower contains more than 93 percent by weight of methyl acetate, the distillate is sent to a methyl acetate hydrolysis device for hydrolysis for obtaining the acetic acid and methanol, the acetic acid is returned to a dehydration tower, the methanol can be used as a fuel for self-use or sale; the para-xylene obtained by absorption from the tail gas is remained at the bottom part of the methyl acetate purifying tower and is returned to a para-xylene oxidation reactor together with discharge port at the bottom part. The method recycles the para-xylene and the methyl acetate in the tail gas and fully utilizes the methyl acetate and the para-xylene obtained by recycling through the methyl acetate purifying tower and the methyl acetate hydrolysis device, thereby significantly reducing the single consumption of para-xylene and acetic acid of the terephthalic acid product, obtaining the methanol by-product and having very significant economic benefits.
Description
Technical field
The present invention relates to organic method in a kind of recycling Production of Terephthalic Acid tail gas, this tail gas comes from the oxidation section in the Production of Terephthalic Acid technology.
Background technology
P-phthalic acid (Purified Terephthalic Acid, be called for short PTA) be the primary raw material of producing polyester fiber and resin, the main at present paraxylene (p-Xylene that adopts, be called for short PX) air oxidation process production, this method is in the PX oxidation reactor, raw material PX is dissolved in the acetic acid-aqueous solvent that contains catalyst acetic acid cobalt, manganese acetate, hydrogen bromide (or tetrabromoethane), and bubbling air or oxygen enrichment carry out oxidation, generate the solid product terephthalic acid (TPA).Typical reaction temperature is 155～205 ℃, pressure 0.6～1.6MPa (absolute pressure), and the time of staying 40～120min, reaction heat shifts out by solvent acetic acid, water evaporation.Give vent to anger and contain a large amount of acetic acid (being called for short HAc), water and nitrogen, unreacted oxygen and a small amount of PX, methyl acetate (being called for short MA), accessory substance CO in the top of PX oxidation reactor
2, CO, CH
3Br.This gas is introduced into dehydrating tower and carries out separating of acetic acid and water, and dehydration overhead condenser (30～40 ℃) does not coagulate the inert gas that gets off and is PTA production tail gas, its pressure 0.6～1.6MPa, and 30～50 ℃ of temperature, composition is mainly N
2, small amount of H
2O and O
2, CO
2, CO, CH
3Br (about 100ppm, ppm is all mass concentration herein), and a small amount of organic matter MA (1000～5000ppm), PX (200～2000ppm), acetic acid (20～200ppm) etc.In some PTA technology, the processing method of PTA being produced tail gas is to be introduced into the decompressor acting, enters regenerative thermal oxide incinerator (RTO) then and purifies, and organic matters such as contained MA, PX, HAc burn into CO in combustion furnace
2, H
2O, CH
3Br is converted into Br
2, final waste gas qualified discharge is to atmosphere, and the RTO operation does not need extraneous postcombustion generally speaking simultaneously, only gets final product with the organic matter that carries in the tail gas.As seen, this processing method, though last waste gas qualified discharge, a large amount of burned burning of organic matter in the tail gas and not being recovered increased the PX and the acetic acid consumption (MA is the PX oxidation reaction by-products, from HAc) of unit mass PTA product.
The exhaust gas treating method that adopts the present invention to propose both can fully have been recycled the organic matter in the tail gas, can guarantee final waste gas qualified discharge again.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, organic method in a kind of recycling Production of Terephthalic Acid tail gas is provided, but organic matters such as PX, MA in this method effective recycling PTA production tail gas, HAc, simultaneously final waste gas also can qualified discharge.
The objective of the invention is to be achieved through the following technical solutions: organic method in a kind of recycling Production of Terephthalic Acid tail gas may further comprise the steps:
(1) Production of Terephthalic Acid tail gas is fed high pressure absorber from the bottom, absorb paraxylene, methyl acetate, acetic acid in the tail gas;
(2) high pressure absorber bottom absorption liquid is delivered to the methyl acetate purifying column, obtain the methyl acetate of high concentration, in tail gas, absorb the paraxylene that obtains and stay methyl acetate purifying column bottom, be back to the p xylene oxidation reactor with bottom discharge;
(3) methyl acetate purifying column top distillate is delivered to the methyl acetate hydrolysis device, methyl acetate hydrolysis is obtained acetic acid and methyl alcohol, acetic acid is back to dehydrating tower;
(4) give vent to anger and go earlier decompressor expansion acting in the high pressure absorber top, goes regenerative thermal oxide incinerator to purify the waste gas qualified discharge after the purification again.
Further, in the described step (1), the operating pressure of described high pressure absorber depends on the pressure of terephthalic acid (TPA) tail gas, is 0.6～1.6MPa.High pressure absorber is the two-part structure, and as cleaning solution, the upper semisection water is as cleaning solution with acetic acid for lower semisection, and the temperature of washing acetic acid and washings is 20～45 ℃.Washing acetic acid can use pure acetic acid, also available dehydrating tower bottom contain aqueous acetic acid more than the acetic acid 90wt%; Washings can be used demineralized water, the extraction water of also available dehydrating tower top return tank.The middle part discharging of high pressure absorber is the acetic acid-water absorption liquid that contains the about 35～65wt% of acetic acid, is back to dehydrating tower to recycle acetic acid.High pressure absorber lower semisection theoretical cam curve is 14～30, and the upper semisection theoretical cam curve is 3～10.
Further, in the described step (2), the number of theoretical plate of described methyl acetate purifying column is 10～25, and reflux ratio is 10～35.The methyl acetate purifying column is an atmospheric operation, and tower top temperature is 57～62 ℃.The methyl acetate purifying column ejects the implication body and be cooled to 10～25 ℃ in overhead condenser.The methyl acetate concentration of methyl acetate purifying column top distillate can reach more than the 93wt%, meets the charging requirement of methyl acetate hydrolysis device.
The invention has the beneficial effects as follows:
1, reclaimed PX, HAc, MA in the PTA tail gas, thereby and densely can deliver to hydrolysis device and made full use of and reclaim the MA that obtains by MA is carried carrying MA after dense;
2, final waste gas qualified discharge;
3, can save the PX consumption 0.6～5kg/tPTA of PTA product per ton, HAc consumes 2～7kg/tPTA, by-product methyl alcohol 1～4kg/tPTA, remarkable in economical benefits.
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Among the figure: 1, PTA tail gas, 2, dehydrating tower, 3, washings, 4, high pressure absorber, 5, decompressor, 6, regenerative thermal oxide incinerator, 7, tail gas emptying, 8, washing acetic acid pump, 9, washing acetic acid cooler, 10, heat exchanger, 11, washing acetic acid, 12, the 1st grade of condenser of methyl acetate purification overhead gas (using recirculated cooling water), 13, the 2nd grade of condenser of methyl acetate purification overhead gas (using chilled water), 14, return tank, 15, the technology scrubbing tower of dropping a hint, 16 methyl acetate hydrolysis devices, 17, reflux pump, 18, the methyl acetate purifying column, 19, reboiler, 20, discharging pump at the bottom of the methyl acetate purifying column, 21, the p xylene oxidation reactor.
The specific embodiment
The present invention recycles that organic method may further comprise the steps in the Production of Terephthalic Acid tail gas:
1, PTA tail gas is fed high pressure absorber 4 from the bottom, to absorb paraxylene, methyl acetate, the acetic acid in the tail gas.
The operating pressure of high pressure absorber 4 depends on the pressure of terephthalic acid (TPA) tail gas, is 0.6～1.6MPa (absolute pressure).High pressure absorber 4 is the two-part structure, lower semisection with the acetum (containing more than the HAc 85wt%) of high concentration as cleaning solution, to absorb PX, the MA oil component in the tail gas; The upper semisection water is as cleaning solution, to absorb the acetic acid that acetic acid in the former tail gas and lower semisection are brought up.The middle part discharging of high pressure absorber 4 is the acetic acid-water absorption liquid that contains the about 35～65wt% of HAc, is back to dehydrating tower 2 to recycle acetic acid.High pressure absorber 4 bottom discharges are mainly acetic acid-aqueous solution, contain MA 0.4～2.0wt%, PX 0.1～0.9wt%.The temperature of washing acetic acid is 20～45 ℃, available pure acetic acid, also available dehydrating tower 2 bottoms contain the above aqueous acetic acid of acetic acid 90wt%; The temperature of washings is 20～45 ℃, available demineralized water, and the extraction water of also available dehydrating tower top return tank often contains certain density MA and HAc in this extraction water.High pressure absorber 4 lower semisection theoretical cam curves are 14～30, and the upper semisection theoretical cam curve is 3～10.Through the PTA tail gas after two sections washings, wherein most MA, PX are absorbed, and high pressure absorber 4 cats head are given vent to anger and contained PX＜100ppm, MA＜400ppm, acetic acid＜200ppm, the CH in the tail gas
3Br is not absorbed substantially, and content still is about 100ppm.In existing some technology, absorption liquid at the bottom of high pressure absorber 4 towers is returned to p xylene oxidation reactor 21 with reuse MA and PX, no doubt do like this and can utilize MA, but do not bring into play the greatest benefit of MA, because this MA major part is oxidized to CO in p xylene oxidation reactor 21
2, CO and having lost.
2, high pressure absorber 4 bottom discharges are delivered to methyl acetate purifying column 18, to obtain the MA (more than the 93wt%) of high concentration; In tail gas, absorb the paraxylene that obtains and stay methyl acetate purifying column 18 bottoms, be back to p xylene oxidation reactor 21 with bottom discharge.
Methyl acetate purifying column 18 is an atmospheric operation, and its number of theoretical plate is 10～25, and reflux ratio is 10～35, and overhead distillate contains MA＞93wt%, PX＜0.5%, H
2O＜5wt%, this distillate meet the charging requirement of methyl acetate hydrolysis device.The operation key of methyl acetate purifying column 18 is to control the PX content of cat head, because overhead MA product will be admitted to the MA hydrolysis device, contained PX can be removed in the MA hydrolysis device and cause PX to lose.The way of PX content is that tower top temperature is controlled at 57～62 ℃ in the control cat head MA product, cat head PX＜0.5%, H under this temperature
2O＜5wt%, thus make that the PX more than 98% stays in 18 end discharging of methyl acetate purifying column in the charging.Methyl acetate purifying column 18 ejects the implication body and is condensed to 10～25 ℃, runs with the MA that the MA condensation is got off, reduced exhaust as far as possible and decreases.This condensation process adopts the series connection of condensed in two stages device to reduce the chilled water consumption, and first order condenser is condensed to 38～50 ℃ with recirculated cooling water, and second level condenser is condensed to 10～25 ℃ with chilled water; Also can adopt one step of single-stage condenser to be condensed to 10～25 ℃.MA purifying column bottom discharge is back to p xylene oxidation reactor 21, to utilize PX wherein.
3, methyl acetate purifying column 18 top distillates are delivered to methyl acetate hydrolysis device 16, methyl acetate hydrolysis obtains acetic acid and methyl alcohol.
In the methyl acetate hydrolysis device 16, the molar yield of methyl acetate hydrolysis product acetic acid or methyl alcohol can reach 95%～99%.Hydrolysis gained acetic acid is the aqueous solution that contains acetic acid 25～55wt%, is back to dehydrating tower to recycle acetic acid; Hydrolysis gained methanol purity can reach 90～99wt%, both can be personal as fuel, also can take out.
4, high pressure absorber 4 top tail gas discharged are gone earlier decompressor 5 expansion actings, go regenerative thermal oxide incinerator (RTO) 6 to purify the tail gas qualified discharge after the purification again.
Organic matter such as residual MA, PX, HAc burns into CO in the tail gas in regenerative thermal oxide incinerator 6
2, H
2O, CH
3Br then is converted into Br
2But the final waste gas qualified discharge after the burning is to atmosphere.For keeping the operation of RTO system, need in RTO, to replenish a certain amount of auxiliary fuel, this auxiliary fuel can be natural gas, methyl alcohol, fuel wet goods gaseous state or liquid fuel, preferred natural gas.
Art methods is promptly removed Production of Terephthalic Acid tail gas to expand without absorption process and is done work, goes then RTO to purify, though do not need additionally to add fuel to RTO, the MA of high value, PX have only served as the role of fuel in the tail gas.As fuel, the calorific value of unit mass natural gas is 2.5 times of MA, 1.2 times of PX, 3.6 times of acetic acid, the price of natural gas is then much lower than MA, PX, the more important thing is that organic content in the tail gas has often surpassed the demand for fuel of RTO, so the economy of prior art scheme is relatively poor.
Compared with prior art, though the present invention needs additionally to add fuel to RTO, but it has reclaimed methyl acetate and the paraxylene in the tail gas, and made full use of by methyl acetate purifying column and methyl acetate hydrolysis device and to have reclaimed methyl acetate and the paraxylene that obtains, thereby significantly reduced the paraxylene of PTA product and acetic acid unit consumption, obtained the methyl alcohol byproduct again, simultaneously still can realize the waste gas qualified discharge, the overall economic efficiency after gains are offset by losses is very remarkable.
The invention will be further described with embodiment with reference to the accompanying drawings below, and it is more obvious that purpose of the present invention and effect will become.
Fig. 1 has provided and has implemented technological process of the present invention, PTA tail gas 1 enters the bottom of high pressure absorber 4, high pressure absorber is last/following two-part structure, the top of lower semisection feeds washing acetic acid 11 to absorb MA and the PX in the tail gas, and the upper semisection top feeds washings 3 to absorb the HAc that gas brings from lower semisection.Washing acetic acid 11 is from dehydrating tower bottom (155 ℃), at first in heat exchanger 10 with absorption tower bottom discharge heat exchange, washing acetic acid is cooled, and discharging then is heated at the bottom of the absorption tower, and washing acetic acid is sent into the top of high pressure absorber lower semisection again by pump 8 after cooler 9 is cooled with circulating water to 40 ℃.The absorption liquid of high pressure absorber upper semisection is an aqueous acetic acid, returns dehydrating tower 2.High pressure absorber top tail gas discharged is gone earlier decompressor 5 expansion actings, goes regenerative thermal oxide incinerator 6 to purify again, last emptying.
The bottom absorption liquid of high pressure absorber enters methyl acetate purifying column 1818 after heating through heat exchanger 10.Giving vent to anger and be condensed to 38～50 ℃ with recirculated cooling water earlier in first order condenser 12 in methyl acetate purifying column 18 tops, enters second level condenser 13 usefulness chilled waters then and be condensed to 10～25 ℃, enters return tank 14 at last.Return tank discharging gas removes the technology scrubbing tower 15 of dropping a hint, and the material in the return tank is sent to methyl acetate hydrolysis device 16 for the MA to high concentration, and hydrolysis gets acetic acid and methyl alcohol, and acetic acid is sent to dehydrating tower 2, and methyl alcohol serves as fuel.Methyl acetate purifying column 18 bottom discharges return PX oxidation reactor 21 for containing the acetum of PX (recovery gained).
Embodiment 1
The exhaust flow 199.9t/h of the PTA device of certain 600,000 tons/a, contain MA=2905ppm, PX=999ppm, tail gas is through behind the high pressure absorber 4, the low absorption liquid of the tower that absorption obtains contains MA 583kg/h (concentration is 1.25wt%), and PX 201kg/h (concentration is 0.429wt%) is behind this absorption liquid process methyl acetate purifying column 1818, finally get MA product 513kg/h (containing MA is 96.5wt%), send to the MA hydrolysis device from the MA overhead; 18 ends of methyl acetate purifying column, contain PX 200kg (concentration is 0.434wt%), is back to the reuse of PX oxidation reactor.Giving vent to anger and be introduced into decompressor and recover energy in the high pressure absorber top, goes RTO to purify again, needs supplemental natural gas 307kg/h in RTO for this reason.Like this, after PTA tail gas is handled by method of the present invention, recyclable MA 513kg/h, the PX 200kg/h of obtaining, can get acetic acid 403kg/h, methyl alcohol 215kg/h (the HAc molar yield of MA hydrolysis calculates by 97%) behind the MA process MA hydrolysis device of 513kg/h, being converted to PTA per ton is acetic acid 5.4kg/tPTA, PX 2.7kg/tPTA, methyl alcohol 2.9kg/tPTA, because organic matter in the tail gas is reclaimed and supplemental natural gas 4.1kg/tPTA.As seen, the MA in the PTA tail gas, PX are fully recycled, and the fuel that supplemental natural gas is moved as RTO in tail gas, MA in the tail gas of both having recycled and PX, reduce the PX and the acetic acid unit consumption of PTA device, can continue to guarantee the tail gas qualified discharge again, the overall economic efficiency highly significant.
High pressure absorber lower semisection absorbent is used for containing the acetic acid 49.9t/h of HAc 89.8wt% bottom dehydrating tower.Because dehydrating tower bottom acetic acid is 155.5 ℃, for guaranteeing assimilation effect, this part acetic acid is reduced to 114 ℃ with absorption liquid at the bottom of the high pressure absorber by heat exchanger 10 heat exchange earlier, is cooled to 40 ℃ by cooler 9 usefulness recirculated cooling waters again, and then advances high pressure absorber; The upper semisection absorbent is used for from the extraction water 6t/h of dehydrating tower top return tank (41 ℃).Absorption liquid is washed acetic acid and is heated to 92 ℃ at the bottom of the high pressure absorber in heat exchanger 10, advances methyl acetate purifying column 1818 again, to make full use of energy.Methyl acetate purifying column 18 top reflux ratios are 17, and tower top temperature is controlled to be 57.2 ℃, and cat head is given vent to anger and is cooled to 45 ℃, is cooled to 20 ℃ with chilled water again with condensed water earlier, run damage the MA condensation is got off, reduced gas phase MA as far as possible; 18 end of methyl acetate purifying column temperature is 114.3 ℃.High pressure absorber ejects gas and contains MA=200ppm, PX=16ppm, HAc=36ppm, CH
3Br=100ppm purifies the back qualified discharge through RTO.
The high pressure absorber diameter is Φ 3400, lower semisection 17m structured packing, and upper semisection is the 316L stainless steel with 15 blocks of valve platies, material.Methyl acetate purifying column 18 diameters are Φ 1400, and 44 valve trays are arranged, and feedboard is the 20th (by the top end of a to counting), and material is 2205 dual phase steels.
Embodiment 2
This example is methyl acetate purifying column 18 embodiments.
For methyl acetate purifying column 18, consider this be one in the water-containing acetic acid system low concentration MA and the separation problem of PX, may relate to the azeotropic entrainment problem of water and PX, water and MA, therefore need test targetedly.For this reason, the inventor specially built one the cover continuous rectifying pilot-plant test.
Methyl acetate purifying column 18 internal diameter Φ 68, the high 1.8m of filler, filler adopt glass spring, and (tower still volume is 10 liters for diameter 4mm, length 5～12mm), and the electrical heating power maximum can reach 2.5KW, and the overhead condenser heat exchange area is 0.3m
2Material enters with the 8kg/h flow continuously from the middle part, consists of HAc=83.91wt%, H
2O=13.10wt%, MA=1.34wt%, PX=1.65wt%, tower top temperature is controlled at 60～61.5 ℃, reflux ratio 17, getting overhead MA concentration after stablizing is 95.7～97.0wt%, PX=0.1～0.5wt%, H
2O=2.5～3.5wt%, the low discharging of tower is that concentration is H
2O=13.5wt%, MA＜0.5wt%.Continuously experiment shows, when temperature is controlled at 57～62 ℃, overhead contains MA＞93wt%, PX＜1wt%, H
2O＜5wt%.Thereby, both obtained meeting the high-purity MA of MA hydrolysis device requirement, again PX has been stayed at the bottom of the tower.
The foregoing description is used for the present invention that explains, rather than limits the invention, and in the protection domain of spirit of the present invention and claim, any modification and change to the present invention makes all fall into protection scope of the present invention.
Claims (1)
1. recycle organic method in the Production of Terephthalic Acid tail gas for one kind, it is characterized in that, may further comprise the steps:
(1) Production of Terephthalic Acid tail gas is fed high pressure absorber from the bottom, absorb paraxylene, methyl acetate, acetic acid in the tail gas;
(2) high pressure absorber bottom absorption liquid is delivered to the methyl acetate purifying column, obtain the methyl acetate of high concentration, in tail gas, absorb the paraxylene that obtains and stay methyl acetate purifying column bottom, be back to the p xylene oxidation reactor with bottom discharge;
(3) methyl acetate purifying column top distillate is delivered to the methyl acetate hydrolysis device, methyl acetate hydrolysis is obtained acetic acid and methyl alcohol, acetic acid is back to dehydrating tower;
(4) give vent to anger and go earlier decompressor expansion acting in the high pressure absorber top, goes regenerative thermal oxide incinerator to purify the waste gas qualified discharge after the purification again;
Wherein, in the described step (2), described high pressure absorber bottom absorption liquid is the acetic acid-aqueous solution that contains methyl acetate 0.4～2.0wt%, contains paraxylene 0.1～0.9wt%; Described methyl acetate purifying column top distillate contains methyl acetate＞93wt%, contains paraxylene＜and 0.5%, moisture＜5wt%; Described methyl acetate purifying column is an atmospheric operation, and tower top temperature is 57～62 ℃; The number of theoretical plate of described methyl acetate purifying column is 10～25, and reflux ratio is 10～35; Described methyl acetate purifying column ejects the implication body and be cooled to 10～25 ℃ in overhead condenser.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP4219407A4 (en) * | 2021-12-07 | 2023-08-23 | Tianhua Institute of Chemical Machinery and Automation Co., Ltd. | System and method for improving water quality of dehydrating tower of purified terephthalic acid apparatus |
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| CN102527186B (en) * | 2012-03-16 | 2014-09-10 | 中石油东北炼化工程有限公司锦州设计院 | Technology and system for recycling solvent oil from oil gas of butadiene prepared from butane under oxidative dehydrogenation effect |
| CN104524929A (en) * | 2015-01-13 | 2015-04-22 | 天津奥展兴达化工技术有限公司 | Efficient energy-saving purification and recovery process of tail gas containing volatile organic compounds (VOCs) |
| CN106178835A (en) * | 2015-05-06 | 2016-12-07 | 中国科学院大连化学物理研究所 | A kind of methylarenes liquid phase oxidation esterification technology for absorbing tail gas |
| CN105344206A (en) * | 2015-11-11 | 2016-02-24 | 天津天清环保科技股份有限公司 | Method and device for processing VOCs in industrial waste gas |
| CN109718634B (en) * | 2017-10-27 | 2022-02-01 | 中国石油化工股份有限公司 | Pretreatment method for waste gas generated by purified terephthalic acid production device |
| CN111408237A (en) * | 2020-03-27 | 2020-07-14 | 焦态成 | Volatile Organic Compounds (VOCs) processing method and device |
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| CN1752060A (en) * | 2005-10-24 | 2006-03-29 | 福州大学 | Recovery method of byproduct methyl acetate in paraphthalic acid production |
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