CN100453146C - Process and apparatus for purifying arene oxidizing tail gas - Google Patents
Process and apparatus for purifying arene oxidizing tail gas Download PDFInfo
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- CN100453146C CN100453146C CNB2006101546070A CN200610154607A CN100453146C CN 100453146 C CN100453146 C CN 100453146C CN B2006101546070 A CNB2006101546070 A CN B2006101546070A CN 200610154607 A CN200610154607 A CN 200610154607A CN 100453146 C CN100453146 C CN 100453146C
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Abstract
The present invention discloses process and apparatus for purifying arene oxidizing tail gas. Two adsorbing beds with filled adsorbent are adopted for alternate adsorption and desorption of organic matter from the tail gas. While one adsorbing bed adsorbs organic matter from the tail gas, the other one desorbs to recover organic matter with compressed air or nitrogen as the desorbing gas and to regenerate the adsorbent, with the desorbed organic matter being returned to the oxidizing system together with the desorbing gas for reuse. The present invention needs no additional desorbed gas treating apparatus and recovers organic matter directly with the tail gas treating apparatus in the oxidizing system, such as condenser, spraying tower, gas waster, etc. The present invention has low adsorption purifying cost and is suitable for industrial use.
Description
Technical field
The present invention relates to a kind of method and apparatus that purifies arene oxidizing tail gas, comprise 2～3 adsorbent beds and relevant adsorption-desorption flow process, be applicable to the purified treatment of tail gas behind the various arene oxidizings and the recycling of organic principle.
Background technology
The liquid phase catalytic oxidation of aromatic hydrocarbons is the various aromatic carboxylic acids of preparation and contains the alcohol of aromatic ring, a class essential industry process of aldehyde compound, for example the paraxylene liquid phase air oxidation prepares terephthalic acid (TPA), meta-xylene oxidation system M-phthalic acid, toluene oxidation system benzoic acid and benzaldehyde, pseudocumene oxidation system trimellitic acid, 2-6 dimethylnaphthalene or 2-6 diisopropyl naphthalene oxidation system 2-6 naphthalenedicarboxylic acid, cumene oxidation system phenol, or the like.These processes all adopt air as oxidant, than higher temperature and pressure (100～250 ℃ are carried out oxidation reaction under 0.5～4.0MP).Owing to contain in the air and do not participate in the inert gas (79% nitrogen) that reacts in a large number, contain many organic principles in the tail gas after the oxidation, comprise raw material, solvent, byproduct of reaction etc., need carry out the recovery and the gas cleaning of organic component, reaching could be to environmental emission after the discharge standard.General oxidized tail gas handling process comprises condensation liquefaction and two polyphones of spray washing unit, most organic in the tail gas can be recycled, but, still contain a small amount of low boiling organic principle in the tail gas and be difficult to remove by said method, make gas not reach discharge standard.Along with the raising day by day of environment protectment protection, how the purified treatment low-concentration organic exhaust gas just becomes the problem of a generality.Current at present way is to add fixed bed of combustion adjuvant (methyl alcohol or natural gas) mixing back feeding to carry out catalytic combustion or degree of depth catalytic oxidation in containing the tail gas of low-concentration organic, discharge after making it change carbon dioxide into, for example the catalytic combustion method introduced of patent WO9611899 and Chinese patent CN1192262.The problem that this method exists is: equipment investment is bigger, needs with noble metal as catalyst; Combustion adjuvant consumption is big, and content of organics is high 4～8 times in the tail gas that its amount ratio is handled; Simultaneously, though this way has been burnt poisonous and hazardous organic principle, increased a lot of CO2 emissions doubly, organic principle does not obtain recycling yet.The common method of another kind of cleaning of off-gas is absorption, adopts adsorbents adsorb organic principles such as active carbon, discharge behind the tail gas clean-up, and reuse behind the adsorbent desorption and regeneration, the gas of desorption is further handled the recovery organic component.It is too high that the subject matter of this method is that desorption reclaims organic cost, after adopting superheated steam or nitrogen desorption, desorption gas also needs to carry out condensation liquefaction, organic principle is removed in the rectifying separation, because organic matter content in desorption gas is not high, the big energy of consumption is used for the processing of desorption gas, when being used for large-scale industrial production, this part investment is just considerable with operating cost, is restricting the widespread usage of this method thus.
Summary of the invention
The object of the invention is to improve the defective of common method for adsorbing and purifying, and a kind of purification method and device of arene oxidizing tail gas of more economical rationality is provided.
For achieving the above object, the present invention has following two kinds of technical solutions.
The purification method of arene oxidizing tail gas adopts the alternately organic matter in absorption and the desorption tail gas of two adsorbent beds that are filled with adsorbent, when the organic component in the adsorbent bed adsorption and oxidation tail gas, another adsorbent bed desorption, desorption gas adopts intrasystem part compressed air, make adsorbent obtain regeneration, the organic matter behind the desorption returns oxidative system with desorption gas and recycles.
The device of employing scheme 1 described arene oxidizing tail gas purification method, comprise oxidation reactor, tail gas heat exchanger, tail gas washing tower, air compressor, the tail gas decompressor, it is characterized in that also having set up two adsorbent beds, the arrival end of two adsorbent beds also connects two pipelines, wherein be connected to first transfer valve and second transfer valve in a pipeline, be connected to the 3rd transfer valve and the 4th transfer valve in another pipeline, between first transfer valve and second transfer valve, there is pipeline to link to each other, has pipeline to link to each other between the 3rd transfer valve and the 4th transfer valve with the air inlet of oxidation reactor with the waste gas outlet of tail gas washing tower; The port of export of two adsorbent beds also connects two pipelines, wherein be connected to the 5th transfer valve and the 6th transfer valve in a pipeline, be connected to the 7th transfer valve and the 8th transfer valve in another pipeline, between the 5th transfer valve and the 6th transfer valve, there is pipeline to link to each other with the air inlet of tail gas decompressor, the pipeline that is located between the 7th transfer valve and the 8th transfer valve is divided into two-way through the 9th valve, one the tunnel connects the gas vent of air compressor, and another road links to each other with the air inlet of oxidation reactor.
The purification method of arene oxidizing tail gas adopts the alternately organic matter in absorption and the desorption tail gas of two adsorbent beds that are filled with adsorbent, when the organic component in the adsorbent bed adsorption and oxidation tail gas, another adsorbent bed desorption, desorption gas adopts intrasystem part nitrogen, make adsorbent obtain regeneration, the organic matter behind the desorption returns oxidative system with desorption gas and recycles.
The device of employing scheme 2 described arene oxidizing tail gas purification methods, comprise oxidation reactor, tail gas heat exchanger, tail gas washing tower, air compressor, the tail gas decompressor, it is characterized in that also having set up two adsorbent beds and a desorption gas wash tower, the arrival end of two adsorbent beds also connects two pipelines, wherein be connected to first transfer valve and second transfer valve in a pipeline, be connected to the 3rd transfer valve and the 4th transfer valve in another pipeline, between first transfer valve and second transfer valve, there is pipeline to link to each other, has pipeline to link to each other between the 3rd transfer valve and the 4th transfer valve with the air inlet of desorption gas wash tower bottom with the waste gas outlet of tail gas washing tower; The port of export of two adsorbent beds also connects two pipelines, wherein be connected to the 5th transfer valve and the 6th transfer valve in a pipeline, be connected to the 7th transfer valve and the 8th transfer valve in another pipeline, between the 5th transfer valve and the 6th transfer valve, there is pipeline to link to each other, has the pipeline heater via to link to each other between the 7th transfer valve and the 8th transfer valve with the gas vent of desorption gas wash tower with the air inlet of tail gas decompressor.
Said desorption can adopt desorption by heating or step-down desorption in above-mentioned two kinds of schemes.Said adsorbent can be activated carbon granule, NACF or silica-rich zeolite.
Beneficial effect of the present invention is:
The present invention adopts the alternately organic matter in absorption and the desorption tail gas of two adsorbent beds that are filled with adsorbent, using system interior section air or nitrogen are as desorption gas, with the organic substance desorption after the absorption, and return oxidative system with desorption gas and recycle, therefore no longer increase desorption gas disposal device, but directly utilize in the oxidative system original exhaust gas processing device such as condenser, spray column, gas scrubbing tower etc. to reclaim organic matter, this just greatly reduces the cost of method for adsorbing and purifying, is convenient to commercial Application.
Description of drawings
Fig. 1 is the process chart of technical solution of the present invention 1;
Fig. 2 is the adsorbent bed schematic diagram that a kind of gas that is filled with solid absorbent flows vertically;
Fig. 3 is the radially mobile adsorbent bed schematic diagram of gas that another kind is filled with solid absorbent;
Fig. 4 is the process chart of technical solution of the present invention 2;
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
With reference to Fig. 1, the device of arene oxidizing tail gas purification method, comprise oxidation reactor 1, tail gas heat exchanger 2, tail gas washing tower 3, air compressor 7, tail gas decompressor 6, two adsorbent beds 4 and 5, the arrival end of two adsorbent beds also connects two pipelines, wherein be connected to first transfer valve 8 and second transfer valve 9 in a pipeline, be connected to the 3rd transfer valve 10 and the 4th transfer valve 11 in another pipeline, between first transfer valve 8 and second transfer valve 9, there is pipeline to link to each other, has pipeline to link to each other between the 3rd transfer valve 10 and the 4th transfer valve 11 with the air inlet of oxidation reactor 1 with the waste gas outlet of tail gas washing tower 3; The port of export of two adsorbent beds also connects two pipelines, wherein be connected to the 5th transfer valve 12 and the 6th transfer valve 13 in a pipeline, be connected to the 7th transfer valve 14 and the 8th transfer valve 15 in another pipeline, between the 5th transfer valve 12 and the 6th transfer valve 13, there is pipeline to link to each other with the air inlet of tail gas decompressor 6, the pipeline that is located between the 7th transfer valve 14 and the 8th transfer valve 15 is divided into two-way through the 9th valve 16, one the tunnel connects the gas vent of air compressor 7, and another road links to each other with the air inlet of oxidation reactor 1.
The selection of adsorbent and the structure of adsorbent bed
The present invention does not have special requirement to adsorbent, all can the highly selective absorption tail gas in the solid absorbent of organic component can both be fit to purposes of the present invention, for example Chang Yong activated carbon granule, activated carbon fiber, silica-rich zeolite etc.
The adsorbent bed that the present invention adopts has two kinds: a kind of is axial packed bed, and referring to Fig. 2, gas enters from an end of bed, exports from the other end; Another kind is a packed bed radially, and referring to Fig. 3, gas enters from the bed center, exports behind peripheral gauge.Axially the advantage of packed bed (Fig. 2) is simple in structure, and cost is low, and subject matter is that the axial length and the diameter ratio of bed is bigger, causes bed pressure drop bigger, can increase the energy consumption of gas dynamic facility (GDF)s such as compressor, decompressor.And radially the stream of packed bed (Fig. 3) gas is shorter, and bed pressure drop is little, and is favourable energy-conservation.
In Fig. 1, air and aromatic hydrocarbons feed oxidation reactor, under higher temperature and pressure, carry out chemical reaction, tail gas enters condenser 2 through offgas duct, scrubbing tower 3 cooling washings, condensate liquid and cleaning solution are sent into other unit of system and are reclaimed, contain a small amount of organic tail gas and enter adsorbent bed 4, be filled with in the adsorbent bed 4 through regeneration, the solid absorbent of high selectivity absorption organic component, tail gas is with after adsorbent contacts, organic component is adsorbed agent absorption under lower temperature and higher pressure, gas is purified, and purified gas is sent into and discharged after tail gas decompressor 6 is recycled energy.Meanwhile, adsorbent bed 5 carries out desorption manipulation, it in the adsorbent bed 5 the saturated organic adsorbent in the tail gas that adsorbed, need carry out desorption and regeneration, regeneration is adopted the higher compressed air of a part of temperature to enter adsorbent bed 5 by side line and is contacted with saturated adsorbent, and it is recycling that organic matter enters oxidation reactor with compressed air behind the desorption from the adsorbent.In the legend, transfer valve 8,10,12,14 is closed condition, and transfer valve 9,11,13,15 is opening, through after certain operating time, adsorbent in the adsorbent bed 4 adsorbance that reaches capacity, adsorbent in the adsorbent bed 5 has been finished regeneration simultaneously, this moment transfer valve 9,11,13,15 close, and transfer valve 8,10,12,14 open, and make tail gas switch to adsorbent bed 5 from adsorbent bed 4, and compressed air switches to adsorbent bed 4 from adsorbent bed 5, two adsorbent bed exchange functions, adsorbent bed 5 adsorbs and adsorbent bed 4 desorptions, and so periodically operation realizes that adsorption-desorption by turns.
With reference to Fig. 4, the device of arene oxidizing tail gas purification method, comprise oxidation reactor 1, tail gas heat exchanger 2, tail gas washing tower 3, air compressor 7, tail gas decompressor 6, it is characterized in that also having set up two adsorbent beds 4,5 and desorption gas wash towers 16, the arrival end of two adsorbent beds also connects two pipelines, wherein be connected to first transfer valve 8 and second transfer valve 9 in a pipeline, be connected to the 3rd transfer valve 10 and the 4th transfer valve 11 in another pipeline, between first transfer valve 8 and second transfer valve 9, there is pipeline to link to each other, has pipeline to link to each other between the 3rd transfer valve 10 and the 4th transfer valve 11 with the air inlet of desorption gas wash tower 16 bottoms with the waste gas outlet of tail gas washing tower 3; The port of export of two adsorbent beds also connects two pipelines, wherein be connected to the 5th transfer valve 12 and the 6th transfer valve 13 in a pipeline, be connected to the 7th transfer valve 14 and the 8th transfer valve 15 in another pipeline, between the 5th transfer valve 12 and the 6th transfer valve 13, there is pipeline to link to each other, has pipeline heater via 17 to link to each other between the 7th transfer valve 14 and the 8th transfer valve 15 with the gas vent of desorption gas wash tower 16 with the air inlet of tail gas decompressor 6.
Here the selection of adsorbent is identical with scheme 1 with the structure of adsorbent bed.
Scheme and Fig. 1 shown in Figure 4 are similar, the desorption gas that the nitrogen that difference is to use in the employing system is used as adsorbent bed 5 desorptions, and the nitrogen of being introduced recycles in system, and system is furnished with and purifies the desorption gas wash tower that reclaims.Adsorbent bed 5 is introduced in the nitrogen heater via 17 intensification backs that come from after the desorption gas wash tower purifies, and the organic matter of adsorbent bed 5 desorptions returns the desorption gas wash tower and reclaims.
The selection of desorption gas and desorption mode
The sweep gas that is used for desorption can have multiple choices, but needs to satisfy two conditions: the one, do not contain the organic component that is adsorbed, and the 2nd, source of the gas is the gas that uses in the system or recycle from oxidative system.Why the source of the gas in the selective system is a device of wishing to utilize original these gases of processing in the system as sweep gas, as compressor, condenser, scrubbing tower or the like, is used to reclaim the organic substance of desorption, thereby does not need to increase extra equipment and expense.When the temperature of compressor outlet gas is higher, be suitable for employing scheme 1 as the reaction end gas purification method; On the other hand, when nitrogen in the system is superfluous, be suitable for employing scheme 2 as the reaction end gas purification method.
The desorption mode of adsorbent bed 5 depends on the selection and the condition of desorption source of the gas.When adopting air as desorption gas, can draw a part from the feed gas pipeline of oxidation reactor, introduce adsorbent bed 5 as side line, take out of behind the organic substance on the adsorbent again with the gas Returning oxidation reactor, as shown in Figure 1, because compressed air temperature is higher, adsorbent bed 5 temperature are higher than adsorbent bed 4, and this desorption mode is a desorption by heating; If select atmospheric air as sweep gas, the exit gas of adsorbent bed 5 enters the suction side of compressor, enters oxidation reactor after the supercharging again, and the pressure of adsorbent bed 5 is lower than the pressure of adsorbent bed 4 in this case, and the desorption mode is exactly the step-down desorption; When the nitrogen that uses in the employing system during as desorption gas, also be according to the temperature of gas and and pressure condition adopt alternating temperature desorption and transformation desorption mode respectively.
The handover operation of absorption and desorption
In order to keep the stable operation of oxidative system, the ratio of the desorption gas of drawing from system is the least possible, so that when desorption manipulation, the switching of gas can not cause the obvious fluctuation of system condition.
Consider the tail gas clean-up problem of terephthalic acid (TPA) (TA) production process, adopt technical scheme shown in Figure 1.Raw material paraxylene (PX) adds oxidation reactor 1 with air and reaction therein generates terephthalic acid (TPA), and reacted tail gas enters condenser 2, scrubbing tower 3 cooling washings from offgas duct, reclaims most of organic principle in the gas; Containing a small amount of organic tail gas enters adsorbent bed 4 and carries out discharging behind the adsorption cleaning.A part of compressed air of drawing from the oxidation reactor air feed pipe enters adsorbent bed 5 by side line desorption tracheae and contacts with saturated adsorbent the bed, and it is recycling to enter oxidation reactor behind the desorption organic matter again.Adsorbent bed 4 regularly switches the adsorption-desorption alternate operation of property performance period with adsorbent bed 5 by transfer valve 8～15.
The production capacity of reactor 1 is 7.5 ten thousand tons of/year TA, and tail gas also contains a small amount of organic matter and is difficult to remove after washing through condensation, needs further remove by adsorption cleaning, and the exhaust flow and the organic matter composition thereof that enter adsorbent bed 4 are listed in table 1.
The flow and the composition of table 1 p xylene oxidation tail gas
Adsorbent bed adopts the activated carbon granule packed bed, and as shown in Figure 2, the relevant adsorbent and the parameter of adsorbent bed 4 are listed in table 2.
Table 2 adsorbent and adsorbent bed 4 operating parameters
The operating parameter of adsorbent bed 5 that is used for desorption is identical with table 2, and desorption gas adopts compressed air, makes adsorbed organic matter desorption from the adsorbent at elevated temperatures, and the flow and the state of desorption gas are listed in table 3.
The sweep gas parameter of table 3 adsorbent bed 2
In the above-described embodiments, by two adsorbent bed alternate operations, organic matter obtains more than 90% recycling in the tail gas, has reached discharge standard behind the tail gas clean-up, behind the organic substance Returning oxidation reactor that reclaims, also has positive role to suppressing the oxidizing process side reaction.In addition, though adsorbent bed 5 adopts compressed air as desorption gas, because organic concentration is lower in the desorption gas, the state of mist is well below burning and blast limit, so that operating process remains is safe.
Consider the tail gas clean-up problem of Production of Terephthalic Acid process, still adopt technical scheme shown in Figure 1.As different from Example 1, adsorbent bed adopts radial bed shown in Figure 3 to reduce bed pressure drop, and simultaneously, adsorbent adopts NACF.The operating parameter of adsorbent and adsorbent bed is listed in table 4, and all the other operating parameters are identical with embodiment 1.
Table 4 adsorbent and adsorbent bed 4 operating parameters
As can be seen from Table 4, NACF specific activity charcoal particle adsorption capacity height, bed pressure drop is low, like this, only needs less adsorbent just can reach same purification purpose.In addition, adopt radial bed to reduce gas, make the bed overall presure drop reduce greatly, help reducing energy consumption by adsorbent bed distance.
Consider the tail gas clean-up problem of Production of Terephthalic Acid process, adopt technical scheme shown in Figure 4, major part and Fig. 1 are similar, difference is that Fig. 4 using system nitrogen is as desorption gas, nitrogen comes from the employed sweep gas of terephthalic acid (TPA) drying machine, from wherein drawing a part, the organic matter of desorption returns 16 recyclings of desorption gas wash tower with gas.Adsorbent bed 4 carries out adsorption operations under higher pressure and lower temperature, the desorption temperature degree that adsorbent bed 5 adopts is higher and pressure is lower, helps desorption manipulation.The operating parameter of adsorbent bed 4 is identical with embodiment 1 or embodiment 2, and the operating parameter of adsorbent bed 5 is listed in table 5.
The sweep gas parameter of table 5 adsorbent bed 5
Claims (2)
1. the purifier of arene oxidizing tail gas, comprise oxidation reactor (1), tail gas heat exchanger (2), tail gas washing tower (3), air compressor (7) and tail gas decompressor (6), it is characterized in that also having set up two adsorbent beds (4) and (5), the arrival end of two adsorbent beds also connects two pipelines, wherein be connected to first transfer valve (8) and second transfer valve (9) in a pipeline, be connected to the 3rd transfer valve (10) and the 4th transfer valve (11) in another pipeline, between first transfer valve (8) and second transfer valve (9), there is pipeline to link to each other, has pipeline to link to each other between the 3rd transfer valve (10) and the 4th transfer valve (11) with the air inlet of oxidation reactor (1) with the waste gas outlet of tail gas washing tower (3); The port of export of two adsorbent beds also connects two pipelines, wherein be connected to the 5th transfer valve (12) and the 6th transfer valve (13) in a pipeline, be connected to the 7th transfer valve (14) and the 8th transfer valve (15) in another pipeline, between the 5th transfer valve (12) and the 6th transfer valve 1 (13), there is pipeline to link to each other with the air inlet of tail gas decompressor (6), the pipeline that is located between the 7th transfer valve (14) and the 8th transfer valve (15) is divided into two-way through the 9th valve (16), one the tunnel connects the gas vent of air compressor (7), and another road links to each other with the air inlet of oxidation reactor (1).
2. the purifier of arene oxidizing tail gas, comprise oxidation reactor (1), tail gas heat exchanger (2), tail gas washing tower (3), air compressor (7) and tail gas decompressor (6), it is characterized in that also having set up two adsorbent beds (4), (5) and a desorption gas wash tower (18), the arrival end of two adsorbent beds also connects two pipelines, wherein be connected to first transfer valve (8) and second transfer valve (9) in a pipeline, be connected to the 3rd transfer valve (10) and the 1 four transfer valve (11) in another pipeline, between first transfer valve (8) and second transfer valve (9), there is pipeline to link to each other, has pipeline to link to each other between the 3rd transfer valve (10) and the 4th transfer valve (11) with the air inlet of desorption gas wash tower (18) bottom with the waste gas outlet of tail gas washing tower (3); The port of export of two adsorbent beds also connects two pipelines, wherein be connected to the 5th transfer valve (12) and the 6th transfer valve (13) in a pipeline, be connected to the 7th transfer valve (14) and the 8th transfer valve (15) in another pipeline, between the 5th transfer valve (12) and the 6th transfer valve (13), there is pipeline to link to each other, has pipeline heater via (17) to link to each other between the 7th transfer valve (14) and the 8th transfer valve (15) with the gas vent of desorption gas wash tower (18) with the air inlet of tail gas decompressor (6).
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| CNB2006101546070A CN100453146C (en) | 2006-11-10 | 2006-11-10 | Process and apparatus for purifying arene oxidizing tail gas |
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| JP2011115709A (en) | 2009-12-02 | 2011-06-16 | Toshiba Corp | Carbon dioxide separating and recovery apparatus |
| CN103055655B (en) * | 2013-01-25 | 2016-04-20 | 浙江曙扬化工有限公司 | A kind of processing method of cyclohexane oxidation system tail gas |
| CN103816764A (en) * | 2013-10-18 | 2014-05-28 | 中国石油化工股份有限公司 | Comprehensive oxidation tail gas utilization method for oxidation process device |
| CN107297140A (en) * | 2016-04-15 | 2017-10-27 | 中国石油化工股份有限公司 | A kind of packaged type exhaust gas processing device and method |
| CN108114574A (en) * | 2016-11-29 | 2018-06-05 | 中国石油化工股份有限公司 | A kind of processing method and processing device of refinery VOCs exhaust gas |
| CN109173582A (en) * | 2018-09-28 | 2019-01-11 | 安徽节源环保科技有限公司 | A kind of processing system of sludge foul gas |
| CN113617185A (en) * | 2021-09-07 | 2021-11-09 | 江苏锦东环境科技有限公司 | Adsorption tower with smooth internal gas circulation |
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Assignee: Yisheng Dahua Petrochemical Co., Ltd. Assignor: Zhejiang University Contract record no.: 2011330001078 Denomination of invention: Process and apparatus for purifying arene oxidizing tail gas Granted publication date: 20090121 License type: Exclusive License Open date: 20070606 Record date: 20110817 |
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