CN103706309A - Reaction rectification reactor - Google Patents
Reaction rectification reactor Download PDFInfo
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- CN103706309A CN103706309A CN201310691574.3A CN201310691574A CN103706309A CN 103706309 A CN103706309 A CN 103706309A CN 201310691574 A CN201310691574 A CN 201310691574A CN 103706309 A CN103706309 A CN 103706309A
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Abstract
The invention discloses a reaction rectification reactor. The reaction rectification reactor comprises a reaction section, a rectification section and a reflux condensation part from bottom to top, wherein a liquid outlet, a gas inlet and a gas distribution plate are arranged on the reaction section from bottom to top; a downspout and the gas distribution plate are arranged in the reactor; the upper end of the downspout is fixed on the gas distribution plate; a liquid inlet is formed in the reactor side wall between the reaction section and the rectification section; holes are evenly formed in the gas distribution plate. Compared with the prior art, the reaction rectification reactor has the beneficial effects that (1) a gas feeding manner of a gas phase is even, the amplitude of fluctuation of a reaction liquid level is small, the liquid level is easily controlled, and the problems of difficult connection between a large-diameter gas inlet pipeline and a gas distributor and processing difficulty of the gas distributor are avoided; (2), one part of reaction heat can be removed by gas carrying a gasified solvent, the temperature is controlled to be stable, and the problems of overheating locally and removing the reaction heat difficultly are avoided; (3), the rectification section and a condenser are capable of better separating certain components which are difficulty separated.
Description
Technical field
The present invention relates to a kind of reactive distillation equipment, especially a kind of reactive distillation reactor.
Background technology
Traditional gas liquid phase reactor is that gas is at liquid phase region bubbling, utilize the dispersed gaseous stream of gas distributor to carry out sufficient gas-liquid mass transfer, distributor form has various ways, and it depends on the many factors such as gas phase state, application scenario, gas phase load, operating pressure, allowable pressure drop, tower diameter.For the condition of production of suitability for industrialized production especially atm number, if distribution of gas is bad, gas phase bubbling can cause the liquid level scope that fluctuates in liquid phase reactor district larger, is unfavorable for that the automation of liquid level is controlled.For atm number, the operating mode of low reaction pressure, gas transmission pipeline diameter can be larger, and for example conventional circular ring type distributor, is being coiled into perforate on the pipe of annulus, this distributor processing, installation and all very difficult with the connected mode of air inlet pipe.In addition, traditional gas liquid phase reactor, normally directly realizes the separation of entrained liquids from liquid phase region bubbling gas out through gas-liquid separator and condenser, for the component of some more difficult separation, is difficult to reach Separation Indexes.
For above situation, those skilled in the art are devoted to study a kind of gas liquid phase reactor of reactive distillation reactor type at present, the reaction of this reactive distillation reactor can be carried out or carry out at rectifying section at tower bottoms phase region, when tower bottoms phase region reacts, relate to equally gas distribution problems with traditional gas liquid phase reactor, when reaction is when rectifying section carries out, be that gas enters from filler below, liquid is from filler top spray, they react in packing section, this mode gas-liquid contact is abundant, but for exothermic reaction, removing of the reaction hot-spot of this mode and reaction heat is a technical barrier.
Summary of the invention
For above problem, the object of this invention is to provide a kind of reactive distillation in conjunction with the reactor carrying out, intake method, structure of reactor are improved, thereby realize and can not need to adopt gas distributor, distribution of gas is effective, reaction zone level stability, and rectifying can realize gas with condensation segment and carries the effective separated of liquid phase component secretly, the local temperature of controlling exothermic reaction is overheated, guarantees that reaction temperature is all even stable.
The present invention is by the following technical solutions:
A kind of reactive distillation reactor, comprise conversion zone, rectifying section and reflux condensation mode section from bottom to top, conversion zone is provided with liquid outlet, air inlet, downspout and gas distribution grid from bottom to top, downspout and gas distribution grid are arranged in reactor, gas distribution grid is fixed in the upper end of downspout, in sidewall of reactor between conversion zone and rectifying section, be provided with inlet, on described gas distribution grid, be provided with perforate, preferably perforate uniformly.
Wherein gas distribution grid is the plate that has perforate, be arranged in reactor, gas enters reactor from the air inlet of gas distribution grid below, by the perforate on gas distribution grid, enter the liquid reactions district on distribution grid on the one hand, when gas is by distribution grid on the other hand, be subject to resistance, this resistance to pressing down, forms wet seal area by the liquid level under sieve plate.Between liquid phase reactor district and wet seal area, be gas zones, we are called distribution of gas space.At present, sieve plate, valve tray, bubble cap tray etc. can be used as gas distribution grid.
Preferably, in above-mentioned reactor, existence for stable maintenance wet seal area and gas distribution space, the hole count of perforate and bore dia on gas distribution grid, according to gas flow and flow relocity calculation, need satisfied requirement to be: when minimum gas flow, this reactor still has distribution of gas space, that is to say: when minimum gas flow, can allow wet seal area, lower end part to flood air inlet, but wet seal area can not be flooded air inlet completely, otherwise gas carries out bubbling stirring completely in wet seal area, break the balance of wet seal area and gas distribution space, thereby cannot form distribution of gas space, but more preferably,, when minimum gas flow, liquid level can, lower than edge under air inlet, guarantee that air inlet is unimpeded.
In above-mentioned reactor, existence for stable maintenance wet seal area and gas distribution space, when air inflow is in busy hour, the gas-phase space height that length of down-comer must can blow out higher than gas, be that length of down-comer will guarantee that lower end can be submerged in wet seal area, thereby avoid downspout unsettled, a part of gas is overflowed from downspout, has broken gas-liquid channel balance.
Preferably, in above-mentioned reactor, the Intensity Design of gas distribution grid is: when reactor shutdowns, distribution grid still can bear the pressure that gathers liquid on distribution grid.
In the liquid flowing away, be dissolved with portion gas downwards in downspout, for the gas in this part liquid that makes to flow in downspout, can from liquid, fully separate with the form of bubble, the flow rate of liquid in downspout is preferably no more than 0.5m/s.
Preferably, for strengthening the stability of downspout, the lower end of downspout can also utilize supporting construction to fix; Supporting construction can be preferably stay pipe or gripper shoe, collar plate shape gripper shoe for example, when using gripper shoe as supporting construction, perforate is preferably set in gripper shoe, so that while there is fluctuation in reaction in reactor, liquid is unlikely to be collected at completely in gripper shoe, increases the load-carrying load of gripper shoe.
Preferably, above-mentioned reflux condensation mode section comprises condenser, when feed liquor amount is less, condenser is preferably directly arranged at tower top, arranging so on the one hand can be when without use liquid distribution trough, liquid also can be evenly distributed on rectifying section, can reduce on the other hand and use condenser one end end socket, has reduced material and the cost of equipment.When feed liquor amount is larger or in the time of may producing liquid flooding, condenser is preferably arranged on tower top one side, preferred horizontal installation.
When air inflow is larger, preferably at air inlet place, impingement baffle is set.
When feed liquor amount is larger, preferably at inlet place, liquid distribution trough is set.Liquid distribution trough can be selected conventional distributor, as pipe distributor, groove type distributor, disc type distributor etc.
Above-mentioned air inlet can be set to one, consider the height arranging in order to reduce gas distribution grid, reduce the height of reactor, reduce material and the cost of reactor, air inlet can be set to a plurality of on the one hand, preferably be symmetricly set in the two side of reactor, for example, be symmetricly set in two air inlets of the two side of reactor.
Preferably, reactor of the present invention also comprises thermometer mouth, liquid level gauge mouth.Thermometer mouth is arranged on liquid phase reactor section, and laying temperature meter is used for monitoring reaction temperature.Liquid level gauge mouth preferably at least arranges two, and wherein at least one is arranged on the liquid phase reactor district of gas distribution grid, and at least one is arranged on wet seal area.According to actual conditions, the liquid level gauge of selecting band to control in the liquid level gauge mouth in liquid phase reactor district, and the liquid level gauge mouth of wet seal area is selected the liquid level gauge that only band shows.
Wherein, the liquid outlet of above-mentioned reactor is arranged at the bottom of reactor.
The present invention fixes a gas distribution grid by the rectifying section in reactor, on distribution grid, have uniform perforate, gas enters the liquid phase reactor district of distribution grid top from the below of distribution grid by the perforate bubbling distribution grid, the resistance that gas runs into when by distribution grid presses down the liquid under distribution grid to form wet seal area, between liquid reactions district and wet seal area, form distribution of gas space, in conversion zone, this spline structure is arranged so that not adopt gas distributor, gas intake method is even, particularly for the larger operating mode of gas phase load, the fluctuating range of reaction liquid level is less, being easy to liquid level controls.
In reactor of the present invention, liquid enters by inlet, liquid phase reactor district with gas on distribution grid reacts, liquid phase reactor gaseous mixture (steam of product and the steam of other volatile materials) out upwards passes through rectifying section, rise to again condenser, part vaporized component is condensed with the steam rising and fully contacts at rectifying section, realize repeatedly part vaporization and the repeatedly vapour-liquid mass of partial condensation between gas-liquid, lower boiling object product is drawn through condensation segment, unreacted and liquid reactants and high boiling product are tackled back conversion zone, high boiling product is drawn by bottom.
Compare with traditional gas-liquid bubbling reactor and reactive distillation reactor, beneficial effect of the present invention is:
(1) reactive distillation reactor of the present invention is for the larger operating mode of gas phase load, gas phase intake method is even, the fluctuating range of reaction liquid level is little, is easy to liquid level and controls, and has also avoided the problem of major diameter admission line with the processing difficulties that is connected difficulty and gas distributor of gas distributor simultaneously.
(2) the present invention's reaction is carried out in liquid phase bubbling area, and rectifying section plays gas liquid separating function, and reaction heat can shift out a part by carried secretly the solvent of gasification by gas, and stable temperature control, does not exist hot-spot and reaction heat to shift out difficult problem.
(3) reaction rectification technique of the present invention is carried gas secretly partially liq by rectifying section and condenser, adds the gas-liquid separation mode of cooler with respect to traditional knockout drum, can better realize the separation of the component of some more difficult separation.
Accompanying drawing explanation
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is the structure of reactor schematic diagram of the embodiment of the present invention 1.
Wherein, 1-downspout gripper shoe; 2-downspout; 3-impingement baffle; 4-sieve plate; 5-liquid phase reactor district, 6-liquid distribution trough, 7-packing support plate, 8-filler, 9-heat exchanger tube, 10-condenser; A-liquid outlet, c1, c2-gas inlet, d-thermometer mouth, q1, q2-liquid phase reactor district liquid level gauge mouth, r1, r2-wet seal area liquid level gauge mouth, n-inlet.
The specific embodiment
Disclosed all features in this description, or the step in disclosed all methods or process, except mutually exclusive feature and/or step, all can combine by any way.
Disclosed arbitrary feature in this description (comprising any accessory claim, summary and accompanying drawing), unless narration especially all can be replaced by other equivalences or the alternative features with similar object.That is,, unless narration especially, each feature is an example in a series of equivalences or similar characteristics.
Embodiment 1
It as shown in Fig. 1, is the structure of reactor schematic diagram of the present embodiment, from the top down, reactor mainly comprises three sections, be respectively reflux condensation mode section, rectifying section and conversion zone, wherein, reflux condensation mode section comprises condenser 10 and heat exchanger tube 9, condenser 10 is directly installed on the tower top of reactor, heat exchanger tube 9 is arranged on inside reactor, it below heat exchanger tube, is rectifying section, this reactor selects the form of packed tower to carry out rectifying, below heat exchanger tube, be filler 8 and for supporting the packing support plate 7 of filler, below packing support plate 7, be provided with liquid distribution trough 6, be arranged in sidewall of reactor with the inlet n being connected with liquid distribution trough 6, inlet place is also provided with impingement baffle 3, below liquid distribution trough 6, be conversion zone, conversion zone comprises sieve plate 4, downspout 2 is connected to the below of sieve plate 4, it is fixing that the lower end of downspout 2 utilizes downspout gripper shoe 1 to support, air inlet c1, c2 is arranged in the sidewall of reactor of sieve plate below, arrange symmetrically one on one side, sieve plate is liquid phase reactor district 5 above, reactant liquor and reactor feed gas are in this region reaction, after unstripped gas is come in from air inlet, from the sieve aperture of sieve plate, enter reaction zone 5, gas is subject to resistance when the sieve aperture by sieve plate, this resistance by the liquid level under sieve plate to pressing down, form wet seal area.At liquid phase reactor district set temperature meter mouth d and two liquid level gauge mouth q1 and q2, two liquid level gauge mouth r1 and r2 are set in wet seal area, the bottom of reactor is provided with liquid outlet a.
Reaction gas 2150kmol/h, 30 ℃ of temperature: pressure 300kPa, reaction gas consists of (v%): N
2: 60.32%, NO:34.72%, O
2: 4.96%, reaction liquid raw material 29100kg/h, temperature 50 C, reactant liquor forms (wt%): alcohol 95 %, water 5%, 50 ℃-70 ℃ of reaction optimum temperatures.It is strict that in the gas product component of this reaction, water content concentration is controlled index request, requires lower than 150ppm.
Reaction equation is: 2 NO+2 C
2h
5oH+1/2O
2→ 2 C
2h
5oNO+H
2o
The present embodiment belongs to the blistering reaction participating in compared with atm number, air inlet duct diameter DN500, the present embodiment is loaded according to rectifying section gas phase, selected tower diameter is 2400mm, because liquid holdup is few, liquid flooding is possibility hardly, so overhead condenser adopts vertical tube-type to be directly installed on tower top, therefore also cut-off footpath 2400mm and tower body one of heat exchanger shell, saving heat exchanger low head.Heat exchange area 913m
2.Packing section is selected metal corrugated packing, height 6m, air inlet mouth of pipe C
1-2dN500, under air inlet, edge is not less than the following 640mm of sieve plate,, plate thickness 5mm, 1250 of sieve apertures, aperture 12mm, equilateral triangle is arranged, downspout Φ 38*3,37, equilateral triangle divides three layers to be evenly distributed on sieve plate, and recycling dry plate resistance calculating peak load is got 1.5 times of normal duty, gets length of down-comer b=1500mm.Liquid phase reactor district liquid level on sieve plate maintains h=2500mm.The pattern n pipe design of liquid distribution trough: length approaches tower internal diameter, 120, Φ 8 hole, minute two rows, angle 90 degree, the hole heart is apart from 40mm.The layout of downspout should guarantee that liquid is no more than 0.1m/s at velocity in pipes.Downspout inserts under the liquid level of the fluid-tight under sieve plate.
Adopt the reactor shown in Fig. 1,62 ℃ of reaction temperature liquid phase region temperature, pressure 300kPa, 6 ℃ of overhead product gas chilling temperatures, flow 2054.87kmol/h, the composition of overhead product gas (v%): ethanol 0.57%, water 0.10%, N
2: 63.11%, NO:15.57%, nitrous ether (ethyl nitrite): 20.64%.
Comparative example 1
In contrast, adopt traditional gas-liquid bubbling reactor to carry out this comparative example's reaction, reaction gas and reaction equation are identical with previous embodiment 1, adopt gas distributor to carry out air inlet, gas product is through gas-liquid separator and cooler, 6 ℃ of cooling rear gas product temperature, flow 2048.16kmol/h, form (v%): ethanol 0.49%, water 0.28%, N
2: 63.32%, NO:15.62%, nitrous ether (ethyl nitrite): 20.30%.
More known, this reaction belongs to the blistering reaction participating in compared with atm number, pipe diameter DN500, and comparative example 1 adopts traditional reactive distillation equipment, and gas distributor pattern is selected and processing difficulties, and the reactor of embodiment 1 does not need to use gas distributor.In addition, the reactor of embodiment 1 can effectively complete the separation of ethanol water, and water content concentration in gas product is reduced as far as possible, meets the requirement of gas product to water content, has compared obvious advantage with traditional gas-liquid separation.
The present invention is not limited to the aforesaid specific embodiment.The present invention expands to any new feature or any new combination disclosing in this manual, and the arbitrary new method disclosing or step or any new combination of process.
Claims (10)
1. a reactive distillation reactor, comprise conversion zone, rectifying section and reflux condensation mode section from bottom to top, it is characterized in that, described conversion zone is provided with liquid outlet, air inlet, downspout and gas distribution grid from bottom to top, described downspout and gas distribution grid are arranged in reactor, gas distribution grid is fixed in the upper end of downspout, in the sidewall of reactor between described conversion zone and rectifying section, is provided with inlet, on described gas distribution grid, is provided with perforate.
2. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, the lower end of described downspout is below the liquid level of wet seal area.
3. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, the intensity of described gas distribution grid for can bear the pressure that gathers liquid on gas distribution grid when reactor shutdowns.
4. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, hole count and the bore dia of described gas distribution grid are set to: when minimum gas flow, described reactor has distribution of gas space.
5. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, the flow rate of liquid in described downspout is no more than 0.5m/s.
6. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, the lower end of described downspout utilizes supporting construction to fix.
7. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, described reflux condensation mode section comprises condenser, and described condenser is arranged at tower top or tower top one side.
8. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, described air inlet place is provided with impingement baffle; Described inlet place is provided with liquid distribution trough.
9. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, described air inlet is set to a plurality of along reactor center line symmetry.
10. a kind of reactive distillation reactor as claimed in claim 1, is characterized in that, also comprises liquid level gauge mouth, thermometer mouth.
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| CN201310691574.3A CN103706309B (en) | 2013-12-17 | 2013-12-17 | A kind of reactive distillation reactor |
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| CN201310691574.3A CN103706309B (en) | 2013-12-17 | 2013-12-17 | A kind of reactive distillation reactor |
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| CN103706309A true CN103706309A (en) | 2014-04-09 |
| CN103706309B CN103706309B (en) | 2015-08-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110785223A (en) * | 2017-06-28 | 2020-02-11 | 环球油品有限责任公司 | Apparatus for vapor-liquid dispensing |
| CN110845321A (en) * | 2019-11-27 | 2020-02-28 | 宿迁南翔化学品制造有限公司 | Tower type method and equipment for preparing malonic acid |
| CN114832738A (en) * | 2021-08-30 | 2022-08-02 | 煤炭科学技术研究院有限公司 | Reactor with a reactor shell |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042664A (en) * | 1988-11-24 | 1990-06-06 | 齐鲁石油化工公司研究院 | Catalytic distillation novel device and antigravity system |
| CN201551865U (en) * | 2009-11-19 | 2010-08-18 | 绍兴市荣发环保科技有限公司 | Rectifying tower |
| CN203620610U (en) * | 2013-12-17 | 2014-06-04 | 西南化工研究设计院有限公司 | Reaction rectification reactor |
-
2013
- 2013-12-17 CN CN201310691574.3A patent/CN103706309B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042664A (en) * | 1988-11-24 | 1990-06-06 | 齐鲁石油化工公司研究院 | Catalytic distillation novel device and antigravity system |
| CN201551865U (en) * | 2009-11-19 | 2010-08-18 | 绍兴市荣发环保科技有限公司 | Rectifying tower |
| CN203620610U (en) * | 2013-12-17 | 2014-06-04 | 西南化工研究设计院有限公司 | Reaction rectification reactor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110785223A (en) * | 2017-06-28 | 2020-02-11 | 环球油品有限责任公司 | Apparatus for vapor-liquid dispensing |
| CN110845321A (en) * | 2019-11-27 | 2020-02-28 | 宿迁南翔化学品制造有限公司 | Tower type method and equipment for preparing malonic acid |
| CN110845321B (en) * | 2019-11-27 | 2022-06-03 | 宿迁南翔化学品制造有限公司 | Tower type method and equipment for preparing malonic acid |
| CN114832738A (en) * | 2021-08-30 | 2022-08-02 | 煤炭科学技术研究院有限公司 | Reactor with a reactor shell |
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| CN103706309B (en) | 2015-08-12 |
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