CN102989187A - Reaction distillation equipment - Google Patents
Reaction distillation equipment Download PDFInfo
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- CN102989187A CN102989187A CN2011102767781A CN201110276778A CN102989187A CN 102989187 A CN102989187 A CN 102989187A CN 2011102767781 A CN2011102767781 A CN 2011102767781A CN 201110276778 A CN201110276778 A CN 201110276778A CN 102989187 A CN102989187 A CN 102989187A
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Abstract
Reaction distillation equipment belongs to the field of distillation equipment in fields of petroleum, chemical engineering and the like. A reaction zone comprises a barrel, a downcomer, a riser and a catch tray; a certain gap is arranged between the downcomer and the catch tray; overflow ports are arranged on the barrel and are higher than the upper part of the gap between the downcomer and the catch tray and lower than a top pipe of the riser. The catalytic distillation equipment for a reaction distillation technology or a catalytic reaction distillation technology has the advantages that the shortcoming of difficultly in control on retention time of liquid in a reaction distillation tower existing in the prior art is overcome, the retention time is conveniently controlled by setting overflow ports with different heights, the retention time of liquid is prolonged according to the need, the retention time of a reactant in the tower can be prolonged to 2h, and the conversion rate of the reactant is increased by more than 80%.
Description
Technical field
The present invention relates to a kind of apparatus for reactive distillation, particularly be suitable for the reactive distillation column that the liquid phase time of staying need to regulate and control, belong to the distillation equipment field of oil, chemical industry etc.
Background technology
The chemical process of traditional catalysis of solid catalyst, carry out catalytic reaction under the effect of liquid phase reacting material solid catalyst in reactor, reacted material enters upstream device, carry out separation of products, for example: product enters in the rectifying column, and overhead product or tower bottom product are as final products or as further refining raw material.Like this, not only technological process is long, equipment investment is large, operating cost is high, and usually because the restriction of chemical balance or cascade reaction etc. have limited the conversion ratio of product and the yield of target product.
In order to overcome the deficiency of traditional chemical process, people have developed reactor and separator is combined in the reactive distillation technology that carries out simultaneously in the equipment.Because reaction is carried out in an equipment simultaneously with separation of products, the product of generation constantly shifts out reaction zone, destroys molecular balance, improves the conversion ratio of reactant; And the reaction be under the bubble point temperature of reactant, to carry out, reaction heat not only controlled reaction temperature, and reaction heat can be used for separation of products by the reaction mass vaporization absorption.Reactive distillation technology has shortened process, reduces equipment investment, reduces the advantage of operating cost.
Reaction in the reactive distillation column is generally carried out in liquid phase, and the control time of staying of liquid in tower is extremely important to the regulation and control reaction effect.For the fast reaction mass of reaction rate, the time of staying of proper extension material in tower, can improve reaction conversion ratio; And for the slow reaction mass of reaction rate, in time shift out the carrying out that reactant that conversion zone generates can accelerated reaction, improve reaction conversion ratio; Therefore the time of staying of the time of staying, the especially reaction product stream of material in the control reactive distillation column that can be convenient and reasonable, extremely important to the regulation and control reaction effect.
Chinese patent ZL01262281, ZL01114953, the liquid phase stream that reaction is generated is collected in the liquid sealing pipe, only have when the liquid level of liquid phase material surpasses the height of liquid sealing pipe downflow weir on one side, liquid phase stream just enters downspout by downflow weir and flows into lower one deck fractionating tray, and the time of staying of liquid phase material in tower can't be controlled easily, and when in the tower downflow weir being set, complicated structure in the tower can not effectively utilize reaction compartment.
The time of staying of material can also be adjusted by changing the methods such as tower tray form, control input and output material flow, adjusting reflux ratio in the present control reactive distillation column, but these method adjustable ranges are little, and not that the internal-response structure of reactive distillation column is made effective adjustment, can't effectively utilize tower internal reaction space.
Summary of the invention
The technical problem to be solved in the present invention: a kind of apparatus for reactive distillation is provided, and this apparatus for reactive distillation can be controlled the time of staying of reaction mass in tower easily, and can effectively utilize tower internal reaction space, improves reaction efficiency.
The technical scheme that product of the present invention is taked is:
Apparatus for reactive distillation of the present invention, the reaction zone of rectifying section or stripping section comprises cylindrical shell, downspout, riser, catch tray, certain slit is arranged between downspout and the catch tray, at cylindrical shell overfall is set, the position of overfall is higher than the upper end in slit between downspout and the catch tray, is lower than the push pipe of riser.
Downspout among the present invention is the inlet pipe of liquid phase material, the pipe that goes out for the reaction liquid product is replaced by the outside pipeline that links to each other with overfall of cylindrical shell, can save like this material and go out pipe in the shared position of reaction zone, and overfall has replaced downflow weir, make simplifying the structure of apparatus for reactive distillation, wherein with in the pipeline that overfall links to each other comprise one section liquid sealing pipe, the length of liquid sealing pipe is determined by the pressure drop of gas phase in the tower, pass through from pipe to prevent gas phase, the shape of overfall can adopt any machinable shape, as square, circular, oval, triangle, pentagon etc.
Length according to liquid phase reacting material needs time of staying in reaction zone can arrange respectively overfall at the cylindrical shell differing heights, and at the sustained height of cylindrical shell an overfall can be set at least.Be connected by pipeline between overfall and the lower one deck tower tray, wherein install pipeline is in the outside of cylindrical shell, the other end of the pipeline that is connected with overfall arranges a liquid distribution trough, and liquid phase stream flows out overfall by piping, then enters uniformly lower one deck plate by liquid distribution trough.Overfall can adopt any machinable shape, such as triangle, circle, square, rectangle etc.
Overfall also can be arranged on the common rectifying tower, can play the effect that reduces liquid residence time.
Further specify below in conjunction with 1 pair of conversion zone of the present invention of accompanying drawing, but application of the present invention is not limited to the apparatus for reactive distillation shown in the accompanying drawing 1.
Conversion zone comprises four parts: catch tray 1, riser 2, downspout 3, overfall 4, cylindrical shell 5, catalyst 6.
The size of catch tray 1 determines that according to the time of staying of liquid phase load and needs its diameter can equal the reactive distillation column tray diameter, also can be greater than tray diameter.Be furnished with riser on the catch tray.
The diameter of riser 2 and quantity are according to the gas phase determination of power load, and its area is generally 3～90% of catch tray area, and the cross sectional shape of riser can be circle, rectangle, square, triangle or other machining shapes.When a riser was only arranged, riser was arranged between two parties, when a plurality of riser is arranged, can adopt rounded projections arranged (such as Fig. 2) or square arrangement (such as Fig. 3).The riser arrangement mode depends on the needs of separation, also is subjected to the impact of catch tray area.The height of riser depends on the height of conversion zone and the height of overfall, and the riser height will be lower than the conversion zone height but be higher than the overfall height.The parts at riser top are baffle plate, the large drop of carrying secretly in order to remove gas, and its shape can be taper.
The liquid material that contains reactant enters conversion zone and reacts through downspout, and liquid level constantly rises on the catch tray, and when reaching the overfall height, liquid leaves the liquid distribution trough that catch tray enters lower one deck tower tray from overfall.Gas enters the catch tray upper space from riser, and namely the gas-phase space of conversion zone leaves conversion zone from the perforate of last layer tower tray again.
As required, for the heterogeneous reaction that has catalyst to exist, can namely be arranged between riser and the riser with in the reaction zone of catalyst arrangement on catch tray, the space between riser and the downspout, between riser and the cylindrical shell.The handling mode of catalyst is mainly determined by catalyst shape, and the heap that can fall apart also can be loaded on catalyst in the member such as screen cloth and is arranged on the catch tray.
Position and the quantity of conversion zone in reactive distillation column is determined by kinetics.As react main rectifying section generation in tower, then conversion zone is arranged in the rectifying section of reactive distillation column.In like manner also can be arranged in the stripping section in the tower.
By reference to the accompanying drawings 5, reactive distillation section and the reaction stripping section of apparatus for reactive distillation of the present invention further specified.
As shown in Figure 5, in the rectifying section of reactive distillation column and stripping section, be respectively arranged with conversion zone.Material enters in the reactive distillation column from charging aperture 14 and separates.Be filled with catalyst 6 on the catch tray 1.The liquid that contains reactant enters the catch tray 1 of conversion zone by downspout 3, and material reacts under the effect of catalyst 6.Gas material enters the upper strata gas-phase space of conversion zone by riser 2.Reacted liquid phase material leaves conversion zone by overfall 4, and the liquid distribution trough 12 that enters lower one deck tower tray through fluid-tight section 13 is reallocated.Reacted liquid phase material flows to the separation tray 11 of bottom, and gaseous phase materials enters last layer separation tray 11, and the reaction that so hockets, the process of separating can meet the requirements of conversion ratio.The vapor-phase material that enters rectifying section after separating from cat head after pipeline 7, condenser 8 condensations, a part is back to cat head through pipeline 10, another part goes out device as light-end products through pipeline 9.The liquid phase material that flow to stripping section goes out tower through pipeline 15 at the bottom of tower after separating, a part is at the bottom of the vapour phase after reboiler 16 vaporizations is returned tower, and another part goes out device as heavy product through pipeline 17.
The difference of embodiment shown in the accompanying drawing 4 and accompanying drawing 5 illustrated embodiment is not have loading catalyst at catch tray 1, and the homogeneous reaction between liquid occurs in the reaction zone of catch tray.
The invention has the beneficial effects as follows: the present invention has overcome the interior liquid residence time shortcoming rambunctious of reactive distillation column in the prior art, has increased operational stability.By different overfall height is set, conveniently the control time of staying, prolong as required liquid residence time, the time of staying of reactant in tower can be increased to 2h, and the conversion ratio of reactant is increased to more than 80%.The present invention is all applicable, applied widely for homogeneous phase and heterogeneous reaction in addition.For heterogeneous reaction, can fully contact with catalyst at reaction zone internal reaction thing, be beneficial to the carrying out of reaction, catalyst efficiency improves.The catalyst centralized arrangement is on catch tray, and catalyst loading and unloading is convenient.
Description of drawings
Fig. 1 is reaction segment structure schematic diagram of the present invention.
Fig. 2 is riser rounded projections arranged schematic diagram in the conversion zone.
Fig. 3 is riser square arrangement schematic diagram in the conversion zone.
Fig. 4 is the reactive distillation column structural representation that is provided with conversion zone.
Fig. 5 is the reactive distillation column structural representation that is provided with conversion zone and is filled with catalyst.
The specific embodiment
Embodiment 1:
Adopt the reactive distillation column separating cracked carbon-5 fraction among Fig. 4.Weight-removing column adopts reactive distillation column shown in Figure 4, can so that the reaction and separation processes process in the single step reaction destilling tower, finish.(chief component is carbon 4 8.4% (mass content to cracking c_5, as follows), pentane 11.6%, amylene 19.2, alkynes 0.2%, isoprene 21.4%, cyclopentadiene 17.2%, pentadiene 13.9%, carbon 6 8.1%, flow is 10000kg/h) enter reactive distillation column, the light components such as isopentane, isoprene comprise that from overhead extraction the material of cyclopentadiene, dicyclopentadiene and pentadiene is from the tower reactor extraction.Reaction distillation column plate number is 70, and C5 fraction is from the 27th plate charging, and reflux ratio is 25, and control tower apical ring pentadiene content is below 1%, and the tower reactor isoprene content is below 1%; 40～65 ℃ of cats head, 0.15～0.3MPa, 80～95 ℃ of tower reactors, 0.3～0.45MPa.Between the 23rd of the rectifying section of reactive distillation column and the 24th block of plate, a conversion zone is set, at stripping section three conversion zones is set, respectively between the 35th and 36 blocks of plates, between the 44th and the 45th, between the 55th and the 56th.In conversion zone, cyclopentadiene generation dimerization reaction generates dicyclopentadiene, and the prolongation of the time of staying is conducive to the carrying out of dimerization reaction.
Each reaction segment structure, measure-alike.2.0 meters of reactive distillation column tower diameters, 2.0 meters of conversion zone diameters, 2.0 meters of conversion zone height.Be furnished with 3 circular riseies on the catch tray, be triangularly arranged, 0.4 meter of draft tube diameter, 1.8 meters of riser height.Cylindrical shell at each conversion zone has 3 overfalls, highly is respectively 1.5 meters, 1.0 meters, 0.5 meter.The time of staying of liquid in 1 conversion zone is 0.3～0.6 hour, can use according to the different demands of reaction the overfall of differing heights.As at the device initial operating stage, close the overfall of 0.5 meter and 1.0 meters height, open the overfall of 1.5 meters height, prolong the time of staying of liquid in tower, to guarantee fully carrying out of dimerization reaction.Carrying out along with reaction, can close 1.5 meters and 0.5m height overfall, open the overfall of 1.0 meters height, along with further carrying out of reaction, close the overfall of 1.5m and 1.0m height, open the overfall of 0.5 meter height, to adjust the time of staying of liquid in tower.Total time of staying of reactive distillation column body of the tower liquid is 1.5～2 hours, and the cyclopentadiene conversion ratio reaches more than 80%, and dicyclopentadiene is selectively greater than 98%.
Embodiment 2:
Adopt reactive distillation column shown in Figure 5 to remove MAPD (propine, allene) in three logistics of cracking carbon.Reactive distillation column is totally 130 blocks of column plates, is mixed with carbon three logistics of hydrogen from the 60th column plate charging.Carbon three logistics feed rates are about 1.5t/h, and MAPD content is about 3.5%, and propylene content is about 92.8%, and surplus is propane.Stripping section at reactive distillation column arranges 4 conversion zones, lays respectively between the 80th and the 81st block of column plate, between the 95th and the 96th block of column plate, between the 110th and the 111st block of column plate, between the 120th and the 121st block of column plate.
Each reaction segment structure, measure-alike in the reactive distillation column.1.0 meters of reactive distillation column diameters, 1.2 meters of conversion zone diameters, 0.55 meter of conversion zone height, a circular riser, 0.5 meter of draft tube diameter, 0.5 meter of the riser height arranged placed in the middle on the catch tray, have three overfalls on each conversion zone, the overfall height is 0.3 meter.Arrange carbon three liquid phase selective hydrogenation catalyst (Beijing Chemical Research Institute's production) at reaction zone, catalyst is spherical, is seated in 10～30 purpose screen clothes, and is stacked in the reaction zone, and catalyst is stacked and highly equaled the overfall height.Liquid is 0.3 hour in the conversion zone time of staying.Liquid total residence time in reactive distillation column is 1.5～2.5 hours, and the conversion ratio of MAPD in tower reaches more than 80%.
Comparative Examples:
In carbon five separation process of prior art, adopt hot dipolymer reactor, make cyclopentadiene generation dimerization reaction generate dicyclopentadiene, then in weight-removing column, dicyclopentadiene and other carbon five components are separated, weight-removing column is common rectifying tower, namely is provided with the conventional structures such as downspout, downflow weir, tower tray perforate, float valve, tower tray in the tower.(chief component is carbon 4 8.4% (mass content in C5 fraction, as follows), pentane 11.6%, amylene 19.2, alkynes 0.2%, isoprene 21.4%, cyclopentadiene 17.2%, pentadiene 13.9%, carbon 6 8.1%, flow are 10000kg/h) through entering weight-removing column after lightness-removing column, the dipolymer reactor, weight-removing column charging chief component is: pentane 8.1%, amylene 18.2%, isoprene 26.1%, cyclopentadiene 3.7%, dicyclopentadiene 17.4%, pentadiene 17.4%, surplus are carbon six.Weight-removing column is common rectifying tower, 110 blocks of column plates, reflux ratio 7.1, liquid phase at dwell time in the tower at 0.1～1 hour.Dimerization reaction occurs in cyclopentadiene hardly in weight-removing column, conversion ratio is very low, below 10%.
Claims (8)
1. apparatus for reactive distillation, reaction zone comprises certain slit between cylindrical shell, downspout, riser, catch tray, downspout and the catch tray, it is characterized in that at cylindrical shell overfall being set, the position of overfall is higher than the upper end in slit between downspout and the catch tray, is lower than the push pipe of riser.
2. apparatus for reactive distillation according to claim 1 is characterized in that reaction zone is arranged on rectification zone or the stripping zone of apparatus for reactive distillation.
3. apparatus for reactive distillation according to claim 1 is characterized in that at the cylindrical shell differing heights overfall being set respectively.
4. apparatus for reactive distillation according to claim 1 is characterized in that at the sustained height of cylindrical shell at least one overfall being set.
5. described any one apparatus for reactive distillation according to claim 1～4 is characterized in that the overfall shape can adopt circle, square, oval, triangle, pentagon.
6. apparatus for reactive distillation according to claim 1 is characterized in that being connected by pipeline between overfall and the lower one deck tower tray, and liquid phase stream flows out overfall and enters lower one deck tower tray by piping.
7. apparatus for reactive distillation according to claim 6 is characterized in that comprising in the pipeline one section liquid sealing pipe, and the length of liquid sealing pipe is determined by the pressure drop of gas phase in the tower.
8. apparatus for reactive distillation according to claim 6 is characterized in that pipeline is in the outside of cylindrical shell.
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| CN201110276778.1A CN102989187B (en) | 2011-09-19 | 2011-09-19 | Reaction distillation equipment |
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| CN201110276778.1A CN102989187B (en) | 2011-09-19 | 2011-09-19 | Reaction distillation equipment |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404848A (en) * | 2018-04-08 | 2018-08-17 | 合润科技有限公司 | A kind of tower plate structure producing polyalphaolefin rectifying column |
| CN110639352A (en) * | 2019-11-02 | 2020-01-03 | 孙发喜 | Vertical multi-stage absorption tower |
| CN110743190A (en) * | 2019-09-25 | 2020-02-04 | 张忠 | Micro-water removing machine in industrial chemical solvent |
| CN112174809A (en) * | 2019-07-05 | 2021-01-05 | 中国石油化工股份有限公司 | Continuous preparation device of homogeneous organic molybdenum compound |
| CN114470839A (en) * | 2022-02-15 | 2022-05-13 | 全椒科利德电子材料有限公司 | High-purity propylene electron gas is heat exchange vary voltage rectification equipment with imitating by force |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108404848A (en) * | 2018-04-08 | 2018-08-17 | 合润科技有限公司 | A kind of tower plate structure producing polyalphaolefin rectifying column |
| CN108404848B (en) * | 2018-04-08 | 2023-09-19 | 合润科技有限公司 | Tower plate structure of rectifying tower for producing poly alpha olefin |
| CN112174809A (en) * | 2019-07-05 | 2021-01-05 | 中国石油化工股份有限公司 | Continuous preparation device of homogeneous organic molybdenum compound |
| CN112174809B (en) * | 2019-07-05 | 2022-10-21 | 中国石油化工股份有限公司 | Continuous preparation device of homogeneous organic molybdenum compound |
| CN110743190A (en) * | 2019-09-25 | 2020-02-04 | 张忠 | Micro-water removing machine in industrial chemical solvent |
| CN110639352A (en) * | 2019-11-02 | 2020-01-03 | 孙发喜 | Vertical multi-stage absorption tower |
| CN110639352B (en) * | 2019-11-02 | 2023-10-20 | 孙发喜 | Vertical multistage absorption tower |
| CN114470839A (en) * | 2022-02-15 | 2022-05-13 | 全椒科利德电子材料有限公司 | High-purity propylene electron gas is heat exchange vary voltage rectification equipment with imitating by force |
| CN114470839B (en) * | 2022-02-15 | 2022-11-11 | 全椒科利德电子材料有限公司 | High-purity propylene electron gas preparation is with high-efficient heat exchange vary voltage rectification equipment |
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