CN102847499A - Quench absorption tower and method for adopting quench absorption tower to absorb methacrolein and methacrylic acid - Google Patents
Quench absorption tower and method for adopting quench absorption tower to absorb methacrolein and methacrylic acid Download PDFInfo
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- CN102847499A CN102847499A CN2012103335807A CN201210333580A CN102847499A CN 102847499 A CN102847499 A CN 102847499A CN 2012103335807 A CN2012103335807 A CN 2012103335807A CN 201210333580 A CN201210333580 A CN 201210333580A CN 102847499 A CN102847499 A CN 102847499A
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Abstract
The invention relates to a quench absorption tower and a method for adopting the quench absorption tower to absorb methacrolein and methacrylic acid. From top to bottom, the quench absorption tower comprises an absorption section, a quenching section, and a tower kettle. The absorption section is composed of the components of a first absorption chamber and a second absorption chamber with distributed perforated baffles, wherein the two chambers are connected in parallel locally with an intermediate perforated separation plate. With the quench absorption tower, isobutylene or tertiary butanol oxidation product gas streams are quenched; methacrolein and methacrylic acid are absorbed; a stream of tail gas on the tower top is delivered to an oxidation reaction system; another stream of tail gas with almost no organic gas such as aldehydes and acid is incinerated and emptied. With the quench absorption tower provided by the invention, methacrolein and methacrylic acid absorption rates are improved; methacrolein recycling rate is improved; and isobutylene or tertiary butanol unit consumption is reduced. Also, the quench absorption tower provided by the invention has high operation flexibility.
Description
Technical field
The present invention relates to a kind of chilled absorbing tower and utilize it to absorb the method for MAL and methacrylic acid.
Background technology
At present, isobutene or Oxidation of t-Butanol prepare the metering system technic acid and mainly concentrate on Japan, oxidation reaction occurs under isobutene or the tert-butyl alcohol and the oxygen high temperature make MAL, and MAL reoxidizes the generation methacrylic acid.
Japan Patent JP2009183817 described oxidation makes in the circulation of tail gas method the oxidation product air-flow that contains MAL and methacrylic acid through a quench tower after, enter again MAL and metering system acid absorption column, because the restriction of absorption tower absorptivity, the tail gas that still contains a certain amount of MAL and methacrylic acid is conveyed to catalytic burning process after, recycle back oxidation unit.Cause thus the loss of a large amount of MALs and methacrylic acid.
Japan Patent JP2005336142 has described quench tower and the absorption tower of MAL and methacrylic acid.Because liquid phase MAL and methacrylic acid are easy to polymerization, chilling and absorption are processed with the tower more than 2 or 2 respectively, and the long meeting of flow process causes pipeline to stop up or equipment scaling reduces assimilation effect, even produce interruption.
The isobutene of existing industrialized unit or Oxidation of t-Butanol are produced the methacrylic acid reaction conversion ratio and are lower than 100%, and absorption plant is lower than 99.96% to the metering system acid absorption rate, and the absorptivity of MAL is lower than 90%.A certain amount of MAL and methacrylic acid have been wasted in the circulation of tail gas process.Cause thus unreacted MAL fully not circulated, greatly increased the consumption of isobutene or the tert-butyl alcohol, limited device metering system acid yield.
Summary of the invention
The invention provides a kind of chilled absorbing tower, this tower is applied in the technique of isobutene or Oxidation of t-Butanol production methacrylic acid, can improve the absorptivity of MAL and methacrylic acid, increase the MAL cyclic utilization rate, absorption plant tail gas has reached the not requirement of passive oxidation catalyst activity simultaneously.Therefore, reduced the isobutene unit consumption, improved the methacrylic acid device capbility, saved production cost simultaneously.
The present invention adopts following technical scheme:
Chilled absorbing tower of the present invention comprises absorber portion, quench zone, tower reactor from top to down, absorber portion is composed in parallel by an absorption chamber and No. two absorption chambers of the baffle of porous baffle that distributing, dividing plate with holes is arranged so that two local series connection of absorption chamber in the middle of an absorption chamber and No. two absorption chambers.
Dividing plate with holes of the present invention is divided into an absorption chamber and No. two absorption chambers with absorber portion, and dividing plate with holes will be divided into two parts perpendicular to the absorber portion diameter R of this plate, perpendicular to the absorber portion diameter R of dividing plate with holes length d at an absorption chamber
1With the length d of absorber portion diameter R at No. two absorption chambers
2Than being 1: 1～7, preferred 1: 1.2～6.7., most preferably 1: 1.5～6.5.
An absorption chamber baffle of porous baffle of the present invention is identical with No. two absorption chamber baffle of porous baffle quantity.
The spacing of baffle of porous baffle of the present invention is two vertical drops of adjacent baffle of porous baffle on dividing plate with holes of same absorption chamber, and No. one absorption chamber baffle of porous baffle spacing is h
1, No. two absorption chamber baffle of porous baffle spacing is h
2, h
1And h
2Identical.
First baffle of porous baffle of an absorption chamber of the present invention is higher or lower than first baffle of porous baffle of No. two absorption chambers, first baffle of porous baffle of an absorption chamber and the vertical drop h of first baffle of porous baffle of No. two absorption chambers on dividing plate with holes
3With h
1Ratio be 0.1～0.3: 1, preferred 0.11～0.29: 1, most preferably 0.12～0.28: 1.
First baffle of porous baffle of an absorption chamber of the present invention and the vertical drop h of first baffle of porous baffle of No. two absorption chambers on dividing plate with holes
3With dividing plate height h ratio with holes be 1: 43～130, preferred 1: 45～127, most preferably 1: 48～121.
Dividing plate height h with holes of the present invention is 9～26: 1 with absorber portion diameter R ratio, preferred 9.3～25.6: 1, most preferably 9.5～25.3: 1.
The angle of an absorption chamber baffle of porous baffle of the present invention and dividing plate with holes is α
1, No. two absorption chamber baffle of porous baffles and dividing plate angle with holes are α
2, α
1=α
2=60 °～120 °, preferred 70 °～110 °, most preferably 75 °～106 °.
First baffle plate of absorber portion of the present invention and dividing plate with holes intersection are to the vertical height h of dividing plate least significant end with holes
4With the ratio of absorber portion diameter R be 0.5～1: 1, preferred 0.53～0.98: 1, most preferably 0.55～0.96: 1.
The hole of an absorption chamber baffle of porous baffle of the present invention, No. two absorption chamber baffle of porous baffles and dividing plate with holes be shaped as rhombus, triangle, circle, ellipse or square.
An absorption chamber baffle of porous baffle hole of the present invention, No. two absorption chamber baffle of porous baffle holes and partition board hole with holes equivalent aperture separately are 1: 1.5～10 with its pitch of holes ratio separately, preferred 1: 2～9, most preferably 1: 2.3～8.
An equivalent aperture, absorption chamber baffle of porous baffle hole of the present invention and No. two absorption chamber baffle of porous baffle hole equivalent aperture ratios are 1～10: 1, preferred 2～9: 1, most preferably 3～8: 1.
Equivalent aperture, No. two absorption chamber baffle of porous baffle holes of the present invention is 1: 330～660 with absorber portion diameter R ratio, preferred 1: 335～655, most preferably 1: 340～650.
The equivalent aperture of partition board hole with holes of the present invention is 1: 50～80 with absorber portion diameter R ratio, preferred 1: 53～78, most preferably 1: 57～75.
Absorber portion diameter R of the present invention is 500～4000mm, preferred 600～3800mm, most preferably 650～3700mm.
Absorber portion diameter R of the present invention is 1: 10～30 with absorber portion height H ratio, preferred 1: 11～28, most preferably 1: 13～26.
Absorber portion of the present invention bottom is cannelure, cannelure external diameter R
1Be absorber portion diameter R, cannelure internal diameter R
2With absorber portion diameter R ratio be 1: 1.5～4, preferred 1: 1.7～3.8, most preferably 1: 2～3.3.
Cannelure inside wall height h of the present invention
5Be 500～3500mm, preferred 520～3400mm, most preferably 550～3200mm.
Cannelure outer wall height h of the present invention
6Be 1000～4000mm, preferred 1100～3800mm, most preferably 1300～3400mm.
Absorber portion of the present invention has identical central shaft with quench zone, the vertical height h of the reducing between absorber portion and the quench zone
7Be 500～2000mm, preferred 530～1800mm, most preferably 550～1500mm.
Absorber portion diameter R of the present invention and quench zone diameter R
3Than being 1: 1～2, preferred 1: 1.1～1.8, most preferably 1: 1.2～1.7.
Quench zone diameter R of the present invention
3With quench zone height h
8Than being 1: 4～10, preferred 1: 4.3～9, most preferably 1: 4.5～8.
Tower reactor diameter R of the present invention
4With quench zone diameter R
3Identical, tower reactor height h
9Be 1000～6000mm, preferred 1050～5800mm, most preferably 1100～5500mm.
The filler that an absorption chamber of the present invention and No. two absorption chambers adopt is the one or two or more of Pall ring filler, ladder ring packing, becket intalox saddle, Tower With Conjugate Rings, θ carbocyclic ring.
The filler equivalent diameter ratio that an absorption chamber of the present invention and No. two absorption chambers adopt is 1～10: 1, preferred 2～9: 1, most preferably 3～8: 1; The equivalent diameter of No. two absorption chamber fillers is 3～180mm, preferred 4～165mm, most preferably 5～150mm.
The filler that quench zone of the present invention adopts is the one or two or more of Pall ring filler, ladder ring packing, becket intalox saddle, Tower With Conjugate Rings, θ carbocyclic ring.
The filler equivalent diameter that quench zone of the present invention adopts is 20～200mm, preferred 25～190mm, most preferably 30～180mm.
Absorber portion packing support plate of the present invention and absorber portion hold-down grid as long as guarantee to satisfy the absorber portion need of work, can be arbitrarily screen.
Quench zone packing support plate of the present invention is fixed between quench zone and the tower reactor, and the quench zone hold-down grid is positioned at quench zone filler top, as long as guarantee to satisfy the quench zone need of work, can be arbitrarily screen.
The present invention also provides in the technique of isobutene or Oxidation of t-Butanol production methacrylic acid and has used described chilled absorbing tower to absorb the method for MAL and methacrylic acid, may further comprise the steps:
A) isobutene or Oxidation of t-Butanol product gas flow enter chilled absorbing tower, after being cooled off by quench liquid, quench zone is divided into two parts, a part is recombinated to divide and is trapped in tower reactor, and the light component that another part contains MAL and metering system acid gas enters absorber portion;
B) light component that contain MAL and metering system acid gas of step in a) enters absorber portion, and MAL and methacrylic acid are absorbed by liquid absorption at absorber portion, are captured in the absorber portion bottom annular recess; The tail gas that is not absorbed by liquid absorption is discharged by the absorber portion top.
Step of the present invention a) in the flow of isobutene or Oxidation of t-Butanol product gas flow be 30～180T/h.
It is 1.5～10.5wt% of oxidation product air flow rate that step of the present invention is trapped in the flow that the restructuring of tower reactor divides in a), and the flow that enters the light component of absorber portion is 89.5～98.5wt% of oxidation product air flow rate.
Step of the present invention a) middle tower reactor liquid level is controlled at based on tower reactor height h
915～95%, preferred 17～91%, most preferably 23～87%.
Step of the present invention a) in the tower reactor temperature at 25～499 ℃, preferred 26～378 ℃, most preferably 28～312 ℃.
Step b of the present invention) absorber portion bottom annular recess liquid level is controlled at based on cannelure inside wall height h in
515～95%, preferred 17～91%, most preferably 23～87%.
Step b of the present invention) absorber portion top exhaust temperature is controlled at 1～99 ℃ in, and preferred 1.1～89 ℃, most preferably 1.3～87 ℃.
Step b of the present invention) restructuring of tower reactor is divided into two stream thighs in, first-class thigh is delivered to restructuring divisional processing system, its flow is 1.5～10.5wt% of oxidation product air flow rate, another stream thigh is with 60～3000T/h, preferred 75～2777T/h, most preferably the flow of 105～2357T/h is sent to the quench zone top and is used for cooling off the oxidation product air-flow that enters chilled absorbing tower as quench liquid.
Step b of the present invention) material that contains MAL and methacrylic acid that is captured in the absorber portion bottom annular recess in is divided into two stream thighs, first-class thigh is delivered to the methacrylic acid refined unit, its flow is 5～19wt% of oxidation product air flow rate, another stream thigh is with 60～3000T/h, preferred 74～2864T/h, most preferably the flow of 92～2462T/h is delivered to the absorber portion top as absorption liquid washing absorption MAL and methacrylic acid after supercooling.
Step b of the present invention) exhaust flow of being discharged by the absorber portion top in is 70.5～93.5wt% of oxidation product air flow rate, be divided into two stream thighs, the first-class strand tail gas that accounts for tail gas total amount 25% is sent into the catalytic burning reactor and is burned, discharge after reaching discharging standards, another stream strand tail gas that accounts for tail gas total amount 75% is compressed to 8～874kpa, preferred 29～457kpa, 45～210kpa most preferably, deliver to oxidation system, control oxidation reaction operating point is outside the blast curve ranges.
Chilled absorbing tower comprises absorber portion, quench zone, tower reactor from top to down, and absorber portion is composed in parallel by an absorption chamber and No. two absorption chambers of the baffle of porous baffle that distributing, dividing plate with holes is arranged so that two local series connection of absorption chamber in the middle of an absorption chamber and No. two absorption chambers.Absorption chamber A unitary gas enters respectively No. two absorption chamber B unit and an absorption chamber C unit after distributing through absorption chamber baffle of porous baffle and dividing plate with holes; No. two absorption chamber B unitary gas enter respectively an absorption chamber C unit and No. two absorption chamber D unit after distributing through No. two absorption chamber baffle of porous baffles and dividing plate with holes.Gas is alternately to contact with two absorption chamber fillers in uphill process.
Because an absorption chamber filler equivalent diameter is greater than No. two absorption chamber filler equivalent diameters, therefore, an absorption chamber filler porosity is greater than No. two absorption chambers, therefore absorption chamber gas handling capacity is large and pressure drop is little, an absorption chamber packing specific area is less than No. two absorption chamber fillers, and No. two absorption chambers of gas-liquid mass transfer area are better than absorption chamber No. one.
Because equivalent aperture, an absorption chamber baffle of porous baffle hole is greater than equivalent aperture, No. two absorption chamber baffle of porous baffle holes, partition board hole equivalent with holes aperture is very large, to such an extent as to any one absorption chamber unit air-flow can pass through dividing plate with holes duct easily, almost without any resistance.Therefore, No. two absorption chamber B unit is suitable with an absorption chamber C unit resistance, and absorption chamber A unitary gas is mean allocation to two absorption chamber B unit and an absorption chamber C unit almost.
Therefore, chilled absorbing tower of the present invention has remedied the absorption tower limitation of using same equivalent diameter filler, well combine the advantage of two kinds of different equivalent diameter fillers by the ingehious design of baffle of porous baffle and dividing plate with holes, improved mass transfer and separative efficiency, reduced simultaneously pressure drop.Metering system acid absorption rate 〉=99.98%, MAL absorptivity 〉=99.90%.
Compared with prior art, the present invention has the following advantages:
1) be coupled preferably chilling and absorb two process functions of chilled absorbing tower disclosed by the invention, absorber portion combines the advantage of sieve plate and filler, has improved mass transfer and separative efficiency.
2) the metering system acid absorption rate of chilled absorbing tower disclosed by the invention is more than 99.98%, the MAL absorptivity is more than 99.9%, the content of MAL and methacrylic acid is low in the tail gas, be recycled in the oxidation unit, not only activity and the life-span of catalyst are not affected, and improved the cyclic utilization rate of MAL, avoid burning the waste that causes, improve the methacrylic acid production capacity, improved economic benefit.
3) chilled absorbing tower disclosed by the invention is easy and simple to handle, has very large operating flexibility.
Description of drawings
Fig. 1 is that isobutene or Oxidation of t-Butanol are produced the methacrylic acid process flow diagram.
Fig. 2 is the structural representation of chilled absorbing tower shown in Figure 1, and wherein, 1 is absorber portion, 2 is quench zone, and 3 is tower reactor, and 4 is quench zone packing support plate, 5 is the quench zone hold-down grid, and 6 is cannelure, and 7 is absorber portion packing support plate, 8 is No. two absorption chamber baffle of porous baffles, 9 is No. two absorption chambers, and 10 is dividing plate with holes, and 11 is the absorber portion hold-down grid, 12 is an absorption chamber, and 13 is an absorption chamber baffle of porous baffle.
Fig. 3 is an absorption chamber shown in Figure 2 and the baffle of porous baffle sectional view of No. two absorption chambers.
Fig. 4 is shown in Figure 2 dividing plate with holes partial section.
The specific embodiment
Below in conjunction with accompanying drawing and instantiation the present invention is made and to describe in further detail.
Fig. 1 is that isobutene or Oxidation of t-Butanol are produced the methacrylic acid process flow diagram, comprises recycled offgas compressor, chilled absorbing tower, quench zone cooler, absorber portion cooler.
Fig. 2 is the structural representation of chilled absorbing tower shown in Figure 1, and wherein, 1 is absorber portion, 2 is quench zone, and 3 is tower reactor, and 4 is quench zone packing support plate, 5 is the quench zone hold-down grid, and 6 is cannelure, and 7 is absorber portion packing support plate, 8 is No. two absorption chamber baffle of porous baffles, 9 is No. two absorption chambers, and 10 is dividing plate with holes, and 11 is the absorber portion hold-down grid, 12 is an absorption chamber, and 13 is an absorption chamber baffle of porous baffle.
Embodiment 1
Produce the methacrylic acid device as example to produce 1.7 ten thousand tons isobutene or Oxidation of t-Butanol per year.
Shown in Fig. 1～4, the chilled absorbing tower that adopts comprises absorber portion 1, quench zone 2, tower reactor 3 from top to down, absorber portion 1 is composed in parallel by an absorption chamber 12 and No. two absorption chambers 9 of the baffle of porous baffle that distributing, dividing plate 10 with holes is arranged so that two local series connection of absorption chamber in the middle of an absorption chamber 12 and No. two absorption chambers 9.Perpendicular to the absorber portion diameter R of dividing plate 10 with holes length d at an absorption chamber 12
1With the length d of absorber portion diameter R at No. two absorption chambers 9
2Than being 1: 3.No. one absorption chamber baffle of porous baffle spacing is h
1Be 3700mm, No. two absorption chamber baffle of porous baffle spacing is h
2Be 3700mm, 12 first baffle of porous baffles of an absorption chamber and the 9 first vertical drop hs of baffle of porous baffle on dividing plate 10 with holes of No. two absorption chambers
3Be 570mm.No. one absorption chamber baffle of porous baffle 13 is identical with No. two absorption chamber baffle of porous baffle 8 quantity.12 first baffle of porous baffles of an absorption chamber are positioned at below 9 first baffle of porous baffles of No. two absorption chambers.1 first baffle of porous baffle of absorber portion and dividing plate with holes 10 intersections are to the vertical height h of dividing plate 10 least significant ends with holes
4Be 1650mm.Dividing plate height h with holes is 28500mm.Absorber portion diameter R is 3000mm.The angle [alpha] of absorption chamber baffle of porous baffle 13 and dividing plate 10 with holes
1Equal the angle [alpha] of No. two absorption chamber baffle of porous baffles 8 and dividing plate 10 with holes
2, all be 85 °.The hole of absorption chamber baffle of porous baffle 13, No. two absorption chamber baffle of porous baffles 8 and dividing plate with holes 10 be shaped as rhombus, absorption chamber baffle of porous baffle hole, No. two absorption chamber baffle of porous baffle holes and partition board hole with holes equivalent aperture separately are respectively 36mm, 5mm and 40mm.Absorption chamber baffle of porous baffle hole, No. two absorption chamber baffle of porous baffle holes and partition board hole with holes equivalent aperture separately are 1: 3 with its pitch of holes ratio separately.The filler that absorption chamber 12 and No. two absorption chambers 9 adopt is the θ carbocyclic ring.The filler equivalent diameter that absorption chamber 12 and No. two absorption chambers 9 adopt is respectively 100mm and 35mm.Absorber portion packing support plate 7 holes be shaped as rhombus, the equivalent aperture is 5mm, the ratio of equivalent aperture and pitch of holes is 1: 3; Absorber portion hold-down grid 11 holes be shaped as rhombus, the equivalent aperture is 5mm, the ratio of equivalent aperture and pitch of holes is 1: 3.The absorber portion height H is 32000mm.Absorber portion 1 bottom is cannelure 6, cannelure external diameter R
1Be 3000mm, cannelure internal diameter R
2Be 1600mm.Cannelure inside wall height h
5Be 610mm, cannelure outer wall height h
6Be 1375mm.The filler that quench zone 2 adopts is Pall ring filler, and equivalent diameter is 150mm.Quench zone packing support plate 4 holes be shaped as rhombus, the equivalent aperture is 100mm, the ratio of equivalent aperture and pitch of holes is 1: 3; Quench zone hold-down grid 5 holes be shaped as rhombus, the equivalent aperture is 100mm, the ratio of equivalent aperture and pitch of holes is 1: 3; Absorber portion 1 has identical central shaft with quench zone 2, the vertical height h of the reducing between absorber portion 1 and the quench zone 2
7Be 1000mm.Tower reactor diameter R
4With quench zone diameter R
3Be all mutually 3600mm, tower reactor height h
9Be 2500mm.Quench zone height h
8Be 18000mm.The load of this chilled absorbing tower is 20.881～45.242T/h.
A) isobutene or Oxidation of t-Butanol product gas flow enter chilled absorbing tower with the flow of 34.80T/h, the oxidation product air-flow is divided into two parts at quench zone 2 by the quench liquid cooling, a part is recombinated to divide and is trapped in tower reactor 3, its flow is 1.59T/h, the light component that another part contains MAL and metering system acid gas enters absorber portion 1, and its flow is 33.21T/h.Be trapped in and be divided into two streams strand after the restructuring lease making over-quenching section heat exchanger cooling of tower reactor 3, first-class thigh is delivered to restructuring divisional processing system, its flow is 1.59T/h, and another stream strand flow with 1209T/h is sent to quench zone 2 tops and is used for cooling off the oxidation product air-flow that enters chilled absorbing tower as quench liquid.Tower reactor 3 liquid levels are controlled at based on tower reactor height h
965%, tower reactor 3 temperature are controlled at 94 ℃.
B) light component that contain MAL and metering system acid gas of step in a) enters absorber portion 1, MAL and methacrylic acid are absorbed by liquid absorption, be captured in absorber portion 1 bottom annular recess 6, material in the cannelure 6 is divided into two stream thighs, first-class thigh is delivered to the methacrylic acid refined unit, its flow is 4.48T/h, delivers to absorber portion 1 top as absorption liquid washing absorption MAL and methacrylic acid after supercooling with the flow of 1030T/h after another stream stock-traders' know-how is crossed the cooling of absorber portion heat exchanger.Absorber portion 1 top exhaust temperature is controlled at 77 ℃.Cannelure 6 liquid levels are controlled at based on cannelure inside wall height h
555%.The tail gas that is not absorbed by liquid absorption is discharged by absorber portion 1 top, its flow is 28.73T/h, be divided into two stream thighs, the first-class strand tail gas that accounts for tail gas total amount 25% is sent into the catalytic burning reactor and is burned, discharge after reaching discharging standards, another stream strand tail gas that accounts for tail gas total amount 75% arrives 88kpa through the recycled offgas compressor compresses, delivers to oxidation system, and control oxidation reaction operating point is outside the blast curve ranges.
Correlation computations formula: absorptivity=(this material is flow-this material flow in tail gas in the oxidation product air-flow) this material of ÷ flow * 100% in the oxidation product air-flow
The results are shown in Table 1:
Table 1 chilled absorbing tower result
The absorptivity of MAL and methacrylic acid is respectively 99.94% and 99.99%, all is higher than absorptivity and the metering system acid absorption rate of existing absorption plant MAL.
Among the embodiment 1, absorption chamber baffle of porous baffle hole, No. two absorption chamber baffle of porous baffle holes and partition board hole with holes equivalent aperture separately change respectively 72mm, 9mm and 50mm into, in addition, the chilled absorbing tower process conditions are identical with embodiment 1, and the chilled absorbing tower absorptivity sees Table 2.
Among the embodiment 1, h
1, h
2And h
3Change into respectively and be 800mm, 800mm and 235mm, in addition, the chilled absorbing tower process conditions are identical with embodiment 1, and the chilled absorbing tower absorptivity sees Table 2.
Among the embodiment 1, the angle [alpha] of absorption chamber baffle of porous baffle 13 and dividing plate 10 with holes
1Equal the angle [alpha] of No. two absorption chamber baffle of porous baffles 8 and dividing plate 10 with holes
2, change 120 ° into, in addition, the chilled absorbing tower process conditions are identical with embodiment 1, and the chilled absorbing tower absorptivity sees Table 2.
Embodiment 5
Among the embodiment 1, perpendicular to the absorber portion diameter of dividing plate 10 with holes length d at an absorption chamber 12
1With the length d of absorber portion diameter at No. two absorption chambers 9
2Than being 1: 6.5, in addition, the chilled absorbing tower process conditions are identical with embodiment 1, and the chilled absorbing tower absorptivity sees Table 2.
The chilled absorbing tower absorptivity result of table 2 embodiment 2～5
Adopt identical with embodiment 1 chilled absorbing tower, feed composition is the same with feed composition in the embodiment table 1, employing different feeds amount, and absorption the results are shown in Table 3.
Table 3 chilled absorbing tower disclosed by the invention under different load to MAL and metering system acid absorption rate
Correction data can be found out from table 3, and when inlet amount was low, chilled absorbing tower disclosed by the invention had extraordinary assimilation effect to MAL and metering system acid absorption rate.Along with the increase of inlet amount, when inlet amount was 45242kg/h, the MAL absorptivity still can reach 99.90%, and the metering system acid absorption rate still can reach 99.98%.Therefore, chilled absorbing tower disclosed by the invention has larger operating flexibility, can reach high-absorbility again simultaneously, and production has significant effect to stabilising arrangement, has brought the Chemical Manufacture stability of height for the client.
Claims (11)
1. chilled absorbing tower, it is characterized in that, described chilled absorbing tower comprises absorber portion (1), quench zone (2), tower reactor (3) from top to down, absorber portion (1) is composed in parallel by an absorption chamber (12) and No. two absorption chambers (9) of the baffle of porous baffle that distributing, and in the middle of an absorption chamber (12) and No. two absorption chambers (9) dividing plate with holes (10) is arranged so that two local series connection of absorption chamber.
2. chilled absorbing tower according to claim 1, it is characterized in that, described dividing plate with holes (10) is divided into an absorption chamber (12) and No. two absorption chambers (9) with absorber portion (1), dividing plate with holes (10) will be divided into two parts perpendicular to the absorber portion diameter R of this plate, perpendicular to the absorber portion diameter R of dividing plate with holes (10) length d at an absorption chamber (12)
1With the length d of absorber portion diameter R at No. two absorption chambers (9)
2Than being 1: 1～7; An absorption chamber baffle of porous baffle (13) is identical with No. two absorption chamber baffle of porous baffles (8) quantity; An absorption chamber baffle of porous baffle spacing h
1With No. two absorption chamber baffle of porous baffle spacing h
2Identical; (12) first baffle of porous baffles of an absorption chamber are higher or lower than (9) first baffle of porous baffles of No. two absorption chambers, (12) first baffle of porous baffles of an absorption chamber and (9) the first vertical drop hs of baffle of porous baffle on dividing plate with holes (10) of No. two absorption chambers
3With h
1Ratio be 0.1～0.3: 1; h
3With dividing plate height h ratio with holes be 1: 43～130; Dividing plate height h with holes is 9～26: 1 with absorber portion diameter R ratio; An absorption chamber baffle of porous baffle (13) is α with the angle of dividing plate with holes (10)
1, No. two absorption chamber baffle of porous baffles (8) are α with the angle of dividing plate with holes (10)
2, α
1=α
2=60 °～120 °; (1) first baffle plate of absorber portion and dividing plate with holes (10) intersection are to the vertical height h of dividing plate with holes (10) least significant end
4With the ratio of absorber portion diameter R be 0.5～1: 1.
3. chilled absorbing tower according to claim 1 and 2, it is characterized in that, the hole of a described absorption chamber baffle of porous baffle (13), No. two absorption chamber baffle of porous baffles (8) and dividing plate with holes (10) be shaped as rhombus, triangle, circle, ellipse or square; Absorption chamber baffle of porous baffle hole, No. two absorption chamber baffle of porous baffle holes and partition board hole with holes equivalent aperture separately are 1: 1.5～10 with its pitch of holes ratio separately; An equivalent aperture, absorption chamber baffle of porous baffle hole and No. two absorption chamber baffle of porous baffle hole equivalent aperture ratios are 1～10: 1; Equivalent aperture, No. two absorption chamber baffle of porous baffle holes is 1: 330～660 with absorber portion diameter R ratio; The equivalent aperture of partition board hole with holes is 1: 50～80 with absorber portion diameter R ratio, and absorber portion diameter R is 500～4000mm.
4. each described chilled absorbing tower is characterized in that according to claim 1～3, and described absorber portion diameter R is 1: 10～30 with absorber portion height H ratio; Absorber portion (1) bottom is cannelure (6), cannelure external diameter R
1Equal absorber portion diameter R, cannelure internal diameter R
2With absorber portion diameter R ratio be 1: 1.5～4; Cannelure inside wall height h
5Be 500～3500mm, cannelure outer wall height h
6Be 1000～4000mm.
5. each described chilled absorbing tower is characterized in that according to claim 1～4, and described absorber portion (1) has identical central shaft with quench zone (2), the vertical height h of the reducing between absorber portion (1) and the quench zone (2)
7Be 500～2000mm; Absorber portion diameter R and quench zone diameter R
3Than being 1: 1～2; Quench zone diameter R
3With quench zone height h
8Than being 1: 4～10; Tower reactor diameter R
4With quench zone diameter R
3Identical, tower reactor height h
9Be 1000～6000mm.
6. each described chilled absorbing tower according to claim 1～5, it is characterized in that the filler of a described absorption chamber (12), No. two absorption chambers (9) usefulness is the one or two or more of Pall ring, cascade ring, metal ring intalox, conjugate ring, θ carbocyclic ring; The filler that quench zone (2) adopts is the one or two or more of Pall ring, cascade ring, metal ring intalox, conjugate ring, θ carbocyclic ring; The filler equivalent diameter ratio that an absorption chamber (12) and No. two absorption chambers (9) adopt is that the equivalent diameter of 1～10: 1, No. two absorption chamber (9) filler is 3～180mm; The filler equivalent diameter that quench zone (2) adopts is 20～200mm.
7. each described chilled absorbing tower of a utilization such as claim 1～6 absorbs the method for MAL and methacrylic acid, may further comprise the steps:
A) isobutene or Oxidation of t-Butanol product gas flow enter chilled absorbing tower, after being cooled off by quench liquid, quench zone (2) is divided into two parts, a part is recombinated to divide and is trapped in tower reactor (3), and the light component that another part contains MAL and metering system acid gas enters absorber portion (1);
B) light component that contain MAL and metering system acid gas of step in a) enters absorber portion (1), MAL and methacrylic acid are absorbed by liquid absorption at absorber portion (1), are captured in absorber portion (1) bottom annular recess (6); The tail gas that is not absorbed by liquid absorption is discharged by absorber portion (1) top.
8. method according to claim 7 is characterized in that, described step a) in the flow of isobutene or Oxidation of t-Butanol product gas flow be 30～180T/h; Being trapped in the flow that the restructuring of tower reactor (3) divides is 1.5～10.5wt% of oxidation product air flow rate, and the flow that enters the light component of absorber portion (1) is 89.5～98.5wt% of oxidation product air flow rate; Tower reactor (3) liquid level is controlled at based on tower reactor height h
915～95%; Tower reactor (3) temperature is controlled at 25～499 ℃; Step b) absorber portion (1) bottom annular recess (6) liquid level is controlled at based on cannelure inside wall height h in
515～95%; Absorber portion (1) top exhaust temperature is controlled at 1～99 ℃.
9. according to claim 7 or 8 described methods, it is characterized in that, the described step a) restructuring of middle tower reactor (3) is divided into two stream thighs, first-class thigh is delivered to restructuring divisional processing system, its flow is 1.5～10.5wt% of oxidation product air flow rate, and another stream strand flow with 60～3000T/h is sent to quench zone (2) top and is used for cooling off the oxidation product air-flow that enters chilled absorbing tower as quench liquid.
10. according to claim 7 or 8 described methods, it is characterized in that, described step b) material that is captured in absorber portion (1) bottom annular recess (6) in is divided into two stream thighs, first-class thigh is delivered to the methacrylic acid refined unit, its flow is 5～19wt% of oxidation product air flow rate, and another stream thigh is delivered to absorber portion (1) top as absorption liquid washing absorption MAL and methacrylic acid with the flow of 60～3000T/h after supercooling.
11. according to claim 7 or 8 described methods, it is characterized in that, described step b) exhaust flow of being discharged by absorber portion (1) top in is 70.5～93.5wt% of oxidation product air flow rate, be divided into two stream thighs, the first-class strand tail gas that accounts for tail gas total amount 25% is sent into the catalytic burning reactor and is burned, discharge after reaching discharging standards, another stream strand tail gas that accounts for tail gas total amount 75% is compressed to 8～874kpa, deliver to oxidation system, control oxidation reaction operating point is outside the blast curve ranges.
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| CN201210333580.7A CN102847499B (en) | 2012-09-04 | 2012-09-04 | Quench absorption tower and method for adopting quench absorption tower to absorb methacrolein and methacrylic acid |
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Cited By (1)
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|---|---|---|---|---|
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