CN102872767B - Industrialized plate type reactor for carbonylating and coupling to synthesize ester - Google Patents
Industrialized plate type reactor for carbonylating and coupling to synthesize ester Download PDFInfo
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- CN102872767B CN102872767B CN201210407063.XA CN201210407063A CN102872767B CN 102872767 B CN102872767 B CN 102872767B CN 201210407063 A CN201210407063 A CN 201210407063A CN 102872767 B CN102872767 B CN 102872767B
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Abstract
The invention relates to an industrialized plate type reactor for carbonylating and coupling to synthesize an ester. A catalyst bed layer of the reactor is internally provided with a gas redistributor; the catalyst bed layer is divided into an outer reaction region and an inner reaction region; a heat exchanging device of the reactor is a heat exchanging plate and a cold pipe, which are prefabricated into a group; the arraying manner of a heat exchanging plate group in the catalyst bed layer is that: the heat exchanging plate group is placed along the radial direction of the catalyst bed layer and is arranged along a concentric vector shape, or is arrayed in a manner of being similar with a concentric circle in a direction which is vertical to the radial direction of the catalyst bed layer. According to the industrialized plate type reactor disclosed by the invention, the disadvantage that the existing reactor for carbonylating and coupling to produce oxalic ester is a tube reactor is overcome, and the disadvantages of the single reactor that the catalyst filling amount is small, the pressure drop is large, large-scale production needs more industrialized plate type reactors and the like can be overcome. The catalyst utilization factor and the reactor capability utilization rate are improved; the catalyst filling amount is increased; the reactor production capability is improved; the device and equipment investment is saved and the operation cost is reduced. The industrialized plate type reactor has good industrialized application effect on a process of carbonylating and coupling to produce the oxalic ester.
Description
Technical field
The present invention relates to a kind of industrialization plate-type reactor that is coupled synthetic ester for carbonylation, relate in particular to a kind of industrialization plate-type reactor that carbonylation is coupled synthesis of oxalate that is applicable to.
Background technology
Oxalate is a kind of important industrial chemicals, can be used for the intermediate of oxalic acid, ethylene glycol, oxamides, medicine and fuel.Particularly along with the minimizing day by day of petroleum resources, by natural gas via synthesis gas, preparing oxalate is a ground-breaking C1 chemical industry new technology, new technology, realize with coal and substitute gas oil ethene, the strategic objective of the indirect synthesizing glycol of two steps, there are very large market prospects, particularly for China's oil resource shortage, and the situation of rich coal resources, this Coal Chemical Industry synthesis of oxalate route has strategic importance.
At present, the fixed bed reactors that carbonylation is coupled synthesis of oxalate adopt shell and tube reactor substantially.Shell and tube reactor is made simple, but is having certain limitation aspect raising respond.Generally, improve respond and mainly by improving heat exchange area and loaded catalyst, solve, namely will strengthen the quantity of diameter or the increase tubulation of tubulation.Can produce like this bed radial temperature profile inhomogeneous, cause reacting wayward, and increase the generation of side reaction.In addition, when power requirement height is to a certain extent time, shell and tube reactor volume is larger, axially and radially larger temperature difference will cause system capacity Efficiency Decreasing, even make the hydrogenation reaction in reactor normally to move.
The reaction that carbonylation is coupled synthesis of oxalate is the mutually reversible catalytic exothermic reaction of gas-solid, for guaranteeing carrying out continuously of heat-producing chemical reaction, need constantly shift out reaction heat, so that course of reaction is carried out along optimum temperature curve.And current industrial employing shell and tube reactor is for the shortcoming such as avoiding catalyst easily aging, service life is short, conventionally adopt in practice a large amount of catalyst of loading, to strengthen reserve factor, the mode of extending catalyst replacement cycle, but too large reserve factor, increase catalyst bed layer height, thereby greatly increased equipment running resistance and power consumption.
In sum, carbonylation is coupled synthesis of oxalate reaction and has following shortcoming at present: the one, adopt pipe type heat transfer structure, and heat transfer coefficient is low, is difficult to realize effectively heat conduction reinforced; The 2nd, hot and cold stream is with the heat exchange of non-full adverse current form, and effectively heat transfer temperature difference is little.Due to the shortcoming of above two aspects, cause existing carbonylation to be coupled synthesis of oxalate inside reactor effective heat exchange area less, consumptive material is many, and equipment manufacturing cost is high, and bulky, and I&M is all inconvenient.In addition, due to the shortcoming of above device structure, make the average reaction temperature in course of reaction lower, cause carbonylation to be coupled synthesis of oxalate reaction rate low, required catalyst amount is many, and equipment investment is high.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, the plate-type reactor that when a kind of gas flow is provided, resistance is little, power consumption is low, callable heat is many, output is high, production cost is low.Solve and overcome the pipe type heat transfer heat transfer coefficient that the inner heat exchange structure of existing hydrogenation reactor exists low, be difficult to realize heat conduction reinforced, the non-full countercurrent flow of hot and cold stream, be that effective heat transfer temperature difference is little, volume is large, installation and maintenance are inconvenient, consumptive material is many, cost is high and average reaction temperature is lower, cause that hydrogenation reaction speed is low, catalyst consumption is large, invest large etc. problem and shortcoming.Board-like gas-solid catalysis device provided by the invention, increased heat transfer coefficient in chamber, strengthened heat transfer, therefore greatly reduced hot(test)-spot temperature, greatly increased catalyst usage factor simultaneously, significantly reduced equipment running resistance and improved the production capacity of installing.
The present invention realizes by the following technical solutions:
For carbonylation, be coupled an industrialization plate-type reactor for synthesis of oxalate, its internal structure comprises Reactor inlet pipe, inlet gas distributor, Heat Room, upper end inert filler layer, intermediate radial reaction bed, lower end inert filler layer, exit gas distributor and the reactor outlet pipe that is positioned at entrance point from top to bottom successively; Described intermediate radial reaction bed, comprises annular space, outer distributing barrel, beds, inside distributor and center discharge between the reactor shell inwall that is connected with upper end inert filler layer and outer distributing barrel from outside to inside successively; In described beds, establish gas redistributor, beds is divided into outer reaction zone and interior reaction zone.
In described beds, establish heat exchanger, the heat exchange element of heat exchanger is plate type heat exchanging element; Described plate type heat exchanging element is prefabricated heat exchanger plates in groups, the plate package being comprised of heat exchanger plates is packed in tower by top manhole, be embedded in beds, plate package integral body supports jointly by being fixed on the annular gusset of reactor shell inwall and center discharge outer wall.
The arrangement mode of described plate package in beds is: be parallel to that beds is radially placed and along concentric fan-shaped arranging, or perpendicular to beds, be radially similar to concentric circles and arrange.The reaction medium of circulation between various heat exchange plate, has different cross-flow modes according to the different in kind of catalyst, and object is to extend the circulation distance of reaction medium between plate, and guarantees that as far as possible each reaction medium circulation path pressure drop approaches identical; Utilize arrange position or be radially similar to concentric circles arrangement position perpendicular to beds of fan-shaped in reaction bed of plate type heat exchanger, can rationally utilize inside reactor heat, vaporization with react between realized good thermal coupling, thereby reach increase heat-transfer effect, raising conversion ratio and object optionally.
When plate package is radially placed and during along concentric fan-shaped arranging, according to the size of the size of reactor inner space and heat exchanger plates itself, radially can be established a heat exchanger plates or establish successively polylith heat exchanger plates along same along beds; Apart from fixing by annular or circular fastening hoop between the heat exchanger plates of reactor axle center same distance.
When plate package is radially similar to concentric circles arrangement perpendicular to beds, same radially heat exchanger plates is arranged in parallel, and the plate package integral body that is positioned at beds is surrounded fixing by being positioned near outer distributing barrel inwall and the outer peripheral circular fastening hoop of plate package; Effective distance between plates between the adjacent heat exchanger plates that same radial parallel is arranged equates.
The heat exchange area of heat exchanger plates is larger than heat exchanger tube, so can take away more reaction heat.And gas is flowed through, and the Area comparison of institute's contact catalyst is large and evenly, reaction combined coefficient is higher.Entire infrastructure is all the standard component of modular, once damage, can be easy to replace.
The thickness of described heat exchanger plates is 0.1～1.0mm.
Described heat exchanger plates is quadrilateral structure, by two metallic plates, is welded, and all heat exchanger plates in same reactor are identical; Two metallic plates of described heat exchanger plates have identical impression, heat exchanger plates hollow, and two metallic plates weld along periphery, surperficial spot welding simultaneously, then punching press is made, the formation fluid passage, gap between two metallic plates.When fluid flows through the plate of above-mentioned impression in crankle mode, accelerated rate of flow of fluid on the one hand, greatly improved overall heat-transfer coefficient, and extended the time that fluid passes through, not only make the reaction of beds gathering in time by the fluid removal of this heat exchanger, make plate inner fluid obtain preheating simultaneously.
Described impression is corrugated, linear, polyline shaped or bubbling shape.
The side that described metallic plate contacts with catalyst is parallel-plate fin structure, and plate wing spacing is 0.1～0.5mm; Adopt described parallel-plate fin structure, can make fluid fully mix and improve heat transfer efficiency in reaction zone, overcome shell and tube reactor limitation in this respect, make structure of reactor compacter simultaneously, bed volume is less, has therefore avoided reactor radial temperature difference and axial temperature difference.
The material of described metallic plate is SS304 metallic plate (gas converting heat plate) or DUPLEX metallic plate (steam heat-exchanging plate), mechanically very firm, good rigidly; SS304 preferably.
The fluid channel design of described plate type heat exchanging element, comprises successively along the flow direction of cooling medium: cooling medium inlet, main distributing pipe, plate package distributing pipe, plate package, heat exchanger plates steam outlet pipe, plate package steam collecting pipe, main collecting pipe and steam outlet pipe mouth.
The process of circulation of cooling medium in described plate type heat exchanging element is: from cooling medium inlet, enter reactor, through main distributing pipe and plate package distributing pipe, enter in the heat exchanger plates of each plate package, after heat exchanger plates and beds heat exchange, produce after low pressure saturated steam collects in heat exchanger plates steam outlet pipe and enter plate package steam collecting pipe, finally, from the low pressure steam of plate package, through main collecting pipe, from steam outlet pipe mouth, discharge reactor and deliver to the external world, carry out follow-up low-pressure steam recycling recycling.
Described cooling medium is boiler feedwater or other cooling fluid, and reaction heat is shifted out to beds in time, produces low-pressure saturated steam simultaneously; Also can gas-gas heat exchange.
In described heat exchanger plates, the type of flow of the outer reactant of cooling medium and plate is cross-flow.
In the outer reaction zone of described beds, establish cold pipe.
Described cold pipe shape of cross section is triangle, square, rhombus or parallelogram; Be preferably triangle.
When plate package is parallel to that beds is radially placed and during along concentric fan-shaped array, described cold pipe, between adjacent two heat exchanger plates apart from reactor axle center same distance, is wedge shape and embeds in beds; To keep effective distance between plates of described adjacent two heat exchanger plates to equate, effective distance between plates of described adjacent two heat exchanger plates is that the distance between described adjacent two heat exchanger plates deducts remaining distance behind the shared space of cold pipe.
When plate package is radially similar to concentric circles arrangement perpendicular to beds, described cold pipe is between the adjacent heat exchanger plates group apart from reactor axle center same distance, being wedge shape embeds in beds, to keep effective distance between plates of described adjacent two plate package to equate, the effective distance between plates between described adjacent plate package is for the distance between adjacent two plate package deducts remaining distance behind the shared space of cold pipe.
In described beds, effective distance between plates of adjacent heat exchanger plates or adjacent heat exchanger plates group is 40～60mm, is preferably 40～50mm.
Medium in described cold pipe is air, unstripped gas, fused salt, water or without medium, is preferably water.
The fluid channel design of described cold pipe, the direction mobile along cooling fluid comprises successively, cold pipe import, cold pipe import distributing pipe, cold pipe, cold pipe exit collector and the outlet of cold pipe.
The process of circulation of cooling fluid in cold pipe is: cooling medium enters from cold pipe import, after cold pipe import distributing pipe distributes, enters each cold pipe, collects, from cold pipe flows out in cold pipe exit collector then from cold pipe outlet outflow reactor.
The inlet gas distributor of described reactor and exit gas distributor, arrange along the perpendicular flow direction of importing and exporting fluid, and on distributor, perforate is arranged and is inverted triangle or parallelogram; Inverted triangle preferably.
Described outer distributing barrel, inside distributor and gas redistributor are cylindrical metal shell, all establish perforate, press the flow direction of fluid, the perforate distribution density in the upstream unit length that flows is larger, and the perforate distribution density in fluid flow downstream unit length is less; Thereby guaranteed being uniformly distributed of air-flow, reduce at dead angle, has improved the utilization rate of catalyst.
Perforate on described outer distributing barrel, inside distributor and gas redistributor is circular, square, triangle, grid or fillet shape; Be preferably fillet shape; On cylinder, perforate is arranged as circumferential or spirality.
Described gas redistributor is redistributed for promoting the circulation of qi body that dissimilar catalyst is separately gone forward side by side.
The catalyst that described outer reaction zone is different with filling in interior reaction zone, described outer reaction zone is away from product equilibrium concentration, reaction motive force is large, per volume of catalyst reaction liberated heat is many, cause in addition reaction zone is the reaction heat concentrated area that carbonylation is coupled synthesis of oxalate reaction, and constantly carrying out along with oxonation in interior reaction zone, gas oxalate content is enrichment gradually, approach product equilibrium concentration, motive force diminishes, it is less that heat is emitted in reaction, therefore need to be suitable for the differential responses enthusiasm condition that inside and outside reaction zone is emitted, shape of catalyst and size in inside and outside reaction zone are carried out to different prioritization schemes, with strengthening reaction diabatic process, make in beds Temperature Distribution rationally and approach optimum temperature curve.
In described outer reaction zone, the particle size of the carbonylation catalyst of filling is 3.2～5.5 * 3.2～5.5mm, is preferably 5 * 5mm.
The shape of carbonylation catalyst comprises cylindrical, Raschig ring, clover, bunge bedstraw herb, the five fingers ball or spherical in described outer reaction zone, is preferably Raschig ring.
In described interior reaction zone, particle size 3.2～5.5 * 3.2～5.5mm of the catalyst of filling, is preferably 3.2 * 3.2mm.
The shape of carbonylation catalyst comprises cylindrical, Raschig ring, clover, bunge bedstraw herb, the five fingers ball or spherical in described interior reaction zone, is preferably the five fingers ball.
The carbonylation catalyst of described beds be placed between heat exchanger plates and heat exchanger plates and heat exchanger plates and cold pipe between space in.
The housing upper end of described plate-type reactor is provided with manhole, lower end is established ring-shaped distributed catalyst and is drawn off the mouth of pipe, under normal service condition, catalyst supports by lower end inert filler bed, when drawing off catalyst, to draw off nozzle flange and lay down, the filler in the catalyst of catalytic bed and bottom inert filler layer draws off mouth of pipe outflow reactor from catalyst.
The process of circulation of reacting gas in described plate-type reactor is: the reacting gas after preheating enters reactor by Reactor inlet pipe, first pass through inlet gas distributor, then further preheating in Heat Room, again through the further uniform distribution of upper end inert filler layer, gas after distribution flows down along annular space between reactor shell inwall and outer distributing barrel, the outer reaction zone that enters beds by the outer distributing barrel of reaction bed radially reacts, and partial reaction gas and reaction product gas enter interior reaction zone and continue reaction after redistributor distributes again; Finally, most product enters center discharge by the inside distributor of reaction bed radially, also have small part directly to enter lower end inert filler layer from the inside distributor of reaction bed radially, then two strands of products pass through exit gas distributor simultaneously, from reactor outlet pipe, flow out.
Described plate-type reactor, for carbonylation, be coupled synthesis of oxalate industrialized unit, but be not limited to " oxidation coupled reaction synthesizing dimethyl oxalate and dimethyl carbonate " reactor that this device also can be used for indication in technological process > > ZL200810043079.0 claim that mono-kind of patent < < produces ethylene glycol with coproduction product dimethyl carbonate, and as the patent No. 201220194360.6, < < acetate is produced the technique > > of ethanol selective coproduction 2-butanols, the acetate hydrogenation reactor of indication in the technique of a patent No. 201210134269.X < < acetate production ethanol selective coproduction 2-butanols and process matched therewith system > > thereof.
The main feature of described plate-type reactor is that heat exchanger plates is inserted in beds, leakes water or other heat transferring medium in plate, and the heat exchange area of heat exchanger plates is larger than heat exchanger tube, so can take away more reaction heat.And gas is flowed through, and the Area comparison of institute's contact catalyst is large and evenly, reaction combined coefficient is higher.Entire infrastructure is all the standard component of modular, once damage, can be easy to replace.Adopt parallel fins plank frame, fluid fully mixes in fan-shaped reaction zone, overcomes shell and tube reactor limitation in this respect, the raising of heat transfer efficiency simultaneously, make structure of reactor compacter, less bed volume, has avoided reactor radial temperature difference and axial temperature difference; Utilize fan-shaped in reaction bed of plate type heat exchanger to arrange position or vertical diameter to concentric circles distributing position, rationally utilize inside reactor heat, vaporization with react between realized good thermal coupling, thereby reach increase heat-transfer effect, raising conversion ratio and object optionally.
Described plate-type reactor fully excavates the potentiality of catalyst, greatly increased catalyst usage factor, equipment running resistance is only 1/6 of shell-and-tube reactor, while heat exchange element, its overall heat-transfer coefficient is more much larger than general heat exchanger, can make reaction heat that catalyst assembles in time by the fluid removal of this plate, have under the characteristic of lower resistance, use plate-type reactor can significantly increase output, easy to make feasible, not only can greatly reduce investment and production cost, but also because thering is automatic mounting, unload the function of carried catalyst, for being coupled the maximization of synthesis of oxalate reactor, current carbonylation started new way, there is good promotion prospect and economic benefit.
Described plate-type reactor, is coupled synthesis of oxalate industrialized unit for carbonylation, is convenient to expansion scale.
Accompanying drawing explanation
A kind of industrialization plate-type reactor internal structure schematic diagram that is coupled synthesis of oxalate for carbonylation of Fig. 1
Fig. 2 is a kind of is coupled for carbonylation in the industrialization plate-type reactor of synthesis of oxalate that plate package is parallel to that beds is radially placed and along concentric fan-shaped array structural representation
The parallel-plate wing structure of Fig. 3 heat exchanger plates and cold pipe partial structurtes elevation
Fig. 4 plate package is parallel to that beds is radially placed and along concentric fan-shaped array local structural graph
Fig. 5 plate package is parallel to that beds is radially placed and along concentric fan-shaped array schematic diagram
Fig. 6 is a kind of to be coupled plate package in the industrialization plate-type reactor of synthesis of oxalate and to be radially similar to concentric circles arrangement architecture schematic diagram perpendicular to beds for carbonylation
Fig. 7 plate package is radially similar to concentric circles perpendicular to beds and arranges local structural graph
Fig. 8 plate package is radially similar to concentric circles perpendicular to beds and arranges schematic diagram
Reference numeral:
1 Reactor inlet pipe
2 inlet gas distributors
3 upper end inert filler layers
4 intermediate radial reaction beds
5 center discharges
6 lower end inert filler layers
7 cooling medium inlets
8 catalyst draw off the mouth of pipe
9 steam outlet pipe mouths
10 main collecting pipes
Annular space between 11 reactor shell inwalls and outer distributing barrel
12 beds
13 exit gas distributors
14 reactor outlet pipes
15 Heat Rooms
16 inside distributors
17 cold pipe imports
18 cold pipe outlets
19 cold pipe exit collectors
20 outer distributing barrels
21 cold pipe inlet distributor
22 main distributing pipes
23 plate package distributing pipes
24 plate package
25 plate wings
26 cold pipe outlet pipes
27 cold pipe cross sections
28 heat exchanger plates steam outlet pipes
29 cold pipes
30 heat exchanger plates
31 fastening hoops
32 reactor shell
33 plate package steam collecting pipes
34 annular gussets
35 gas redistributors
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can do any change or modification to the present invention after having read the content that the present invention tells about, these equivalent form of values fall within the application's appended claims limited range equally.
The experimental technique of unreceipted actual conditions in embodiment below, conventionally according to normal condition, as: chemical industry operation handbook, or the condition of advising according to manufacturer.
The industrialization plate-type reactor (carrying out carbonylation coupled reaction) of 300,000 tons of oxalates of annual output as shown in Figure 1 and Figure 2, internal diameter 4.0m, (T.L) 12.0m highly, synthesis pressure 0.2MPa; Its internal structure comprises Reactor inlet pipe 1, inlet gas distributor 2, Heat Room 15, upper end inert filler layer 3, intermediate radial reaction bed 4, lower end inert filler layer 6, exit gas distributor 13 and the reactor outlet pipe 14 that is positioned at entrance point from top to bottom successively; Described intermediate radial reaction bed 4, comprises annular space 11, outer distributing barrel 20, beds 12, inside distributor 16He center discharge 5 between reactor shell 32 inwalls that are connected with upper end inert filler layer 3 and outer distributing barrel from outside to inside successively; In described beds 12, establish gas redistributor 35, beds 12 is divided into outer reaction zone and interior reaction zone.
In described beds, 12 establish heat exchanger, and the heat exchange element of heat exchanger is plate type heat exchanging element; Described plate type heat exchanging element is prefabricated heat exchanger plates 30 in groups, it is long that monolithic heat exchanger plates 30 is of a size of 7m() x0.4m(is wide), the plate package 24 being comprised of heat exchanger plates 30 is packed in tower by top manhole, be embedded in beds 12, plate package 24 integral body support jointly by being fixed on the annular gusset 34 of reactor shell 32 inwalls and center discharge 5 outer walls.
The quadrilateral structure that described heat exchanger plates 30 is made for automation, is welded by two SS304 metallic plates, and in same reactor, all heat exchanger plates 30 are identical; Two metallic plates have identical bubbling shape impression, heat exchanger plates 30 hollows, and two metallic plates weld along periphery, surperficial spot welding simultaneously, then punching press is made, the formation fluid passage, gap between two metallic plates; The side that metallic plate contacts with catalyst is parallel-plate fin structure, and plate wing 25 spacing are 0.1～0.5mm.
The arrangement mode of described plate package 24 in beds 12 is: be parallel to that beds 12 is radially placed and along concentric fan-shaped arranging; Along same, radially establish 3 heat exchanger plates 30; Apart from fixing by circular fastening hoop 31 between the heat exchanger plates 30 of reactor axle center same distance.
The fluid channel design of the plate type heat exchanging element of described plate-type reactor, comprises successively along the flow direction of cooling medium: the import 7 of cooling medium, main distributing pipe 22, plate package distributing pipe 23, plate package 24, heat exchanger plates steam outlet pipe 28, plate package steam collecting pipe 33, main collecting pipe 10 and steam outlet pipe mouth 9.
Outer reaction zone along described beds 12 is established cold pipe 29 away from center discharge 5 places between two the adjacent heat exchanger plates 30 apart from reactor axle center same distance, be wedge shape and embed beds 12, cold pipe cross section 27 is shaped as triangle, effective distance between plates apart from 30 of adjacent two heat exchanger plates of reactor axle center same distance is 40mm, guarantee catalyst radially tangent plane filling overall width be 40mm.In space between the heat exchanger plates 30 of beds 12 and heat exchanger plates 20 and between heat exchanger plates 30 and cold pipe 29, filling is coupled the catalyst of synthesis of oxalate for carbonylation.During reaction, logical supercooling tube 29 is taken away unnecessary beds 12 heat of reaction by indirect heat exchange, take and guarantees that outer reaction zone beds 12 Temperature Distribution are as optimal temperature distribution.
The channels designs of described cold pipe 29, the direction mobile along cooling fluid comprises successively, cold pipe import 17, cold pipe import distributing pipe 21, cold pipe 29, cold pipe exit collector 19 and cold pipe outlet 26.
Described inlet gas distributor 2 and exit gas distributor 13, along the perpendicular flow direction setting of reacting gas, on distributor, perforate is arranged as del.
Described outer distributing barrel 20, inside distributor 16 and gas redistributor 35 are cylindrical metal shell, all establish perforate on it, and hole shape is fillet shape, and perforate is circumferential arrangement; Press the flow direction of fluid, the perforate distribution density flowing in the unit length of upstream in fluid is larger, and the perforate distribution density in fluid flow downstream unit length is less, thereby has guaranteed being uniformly distributed of air-flow, reduce at dead angle, has improved the utilization rate of catalyst.Described inside distributor 16 diameters are 0.85m, and described outer distributing barrel 20 diameters are 3.8m; The diameter of described gas redistributor 35 is 1.9m.
The dissimilar carbonylation catalyst of filling in described outer reaction zone and interior reaction zone; In described outer reaction zone, the carbonylation catalyst of filling is shaped as Raschig ring, and particle size is 5 * 5mm; In described interior reaction zone carbonylation catalyst be shaped as the five fingers ball, particle size is 3.2 * 3.2mm.
The lower end of described plate-type reactor is established the catalyst of apportion in the form of a ring and is drawn off the mouth of pipe 8, under normal service condition, catalyst supports by reactor lower end inert filler layer 6, when drawing off catalyst, catalyst is drawn off to the mouth of pipe 8 flanges and lay down, the filler of the catalyst of beds 12 and lower end inert filler layer 6 draws off the mouth of pipe 8 outflow reactors from catalyst.
In heat exchanger plates 30, walk boiler feedwater (CL
-be less than 4PPM), from cooling medium inlet 7, enter reactor, through main distributing pipe 22, enter in each plate package 24, then after plate package distributing pipe 23, enter in the heat exchanger plates 30 of each plate package 24, after heat exchanger plates 30 and catalyst heat exchange, produce after low pressure saturated steam collects in heat exchanger plates steam outlet pipe 28 and enter plate package steam collecting pipe 33, finally, from the low pressure steam of plate package 24, through main collecting pipe 10, from steam outlet pipe mouth 9, discharge reactor and deliver to extraneous recycling, sending water vapour pressure outside is 0.3～0.5MPa.
In cold pipe 29, also walk boiler feedwater, the logical supercooling tube import 17 of boiler feedwater and cold pipe inlet distributor 21 enter the cold pipe 29 that is positioned at beds 12, the unnecessary heat of reaction of beds 12 is taken away by indirect heat exchange, then after collecting, cold pipe exit collector 19 discharges reactor from cold pipe outlet 18, logical like this supercooling tube 29 auxiliary heat-exchangings be take and guaranteed that outer reaction zone beds 12 Temperature Distribution distribute as optimal temperature, thereby guarantee that the high conversion of catalyst, with selective, improves catalyst usage factor.
While carrying out carbonylation coupled reaction, mist (105 ℃ of temperature, pressure 0.2MPa) first from tower top Reactor inlet pipe 1, by inlet gas distributor 2, enter upper end inert filler layer 3, to strengthen distribution of gas, Heat Room 15 interior through further with steam indirect heat exchange after and after gas phase redistribution, mixing temperature reaches 140 ℃, along reactor shell 32 inwalls and 20 annular spaces 11 of outer distributing barrel, flow down, by the outer distributing barrel 20 of reaction bed 4 radially, enter the outer reaction zone of beds 12, outer reaction zone beds 12 temperature are controlled at 120～130 ℃, reaction conversion ratio 50%, dimethyl oxalate selective 70%, under the catalyst shape acting in conjunction of reaction heat due to good plate heat transfer efficiency and larger catalyst granules and hollow, shifted out rapidly, avoided the accumulation of heat, thereby guaranteed that reaction bed does not become high focus.Then reacting gas and reaction product gas together enter the interior reaction zone continuation reaction of beds 12 after redistributor 35 redistributions, and interior reaction zone temperature is controlled at 130～140 ℃, reaction conversion ratio 85%, dimethyl oxalate selective 94%.Qualified thick oxalate is produced in now reaction, and it is 135 ℃ that material goes out temperature of reactor.Finally, most of product enters center discharge 5 from inside distributor 16, also has small part directly to enter lower floor's inert filler layer 6 from inside distributor 16, and then two strands of products pass through exit gas distributor 13 simultaneously, from reactor outlet pipe 14, flow out, reaction bed pressure is reduced to 0.06MPa.
Described plate-type reactor can obtain more massive reaction unit by the size of increase unit process body or the quantity of increase unit process body.This is just different from the too huge shortcoming of volume after shell and tube reactor expansion scale.
Claims (12)
1. one kind is coupled the industrialization plate-type reactor that synthesizes ester for carbonylation, it is characterized in that, comprise successively from top to bottom the Reactor inlet pipe (1), inlet gas distributor (2), Heat Room (15), upper end inert filler layer (3), intermediate radial reaction bed (4), lower end inert filler layer (6), exit gas distributor (13) and the reactor outlet pipe (14) that are positioned at entrance point; Described intermediate radial reaction bed (4), comprises annular space (11), outer distributing barrel (20), beds (12), inside distributor (16) and center discharge (5) between reactor shell (32) inwall that is connected with upper end inert filler layer (3) and outer distributing barrel (20) from outside to inside successively; In described beds (12), establish gas redistributor (35), beds (12) is divided into outer reaction zone and interior reaction zone;
Described beds is established heat exchanger in (12), and the heat exchange element of heat exchanger is plate type heat exchanging element; Described plate type heat exchanging element is prefabricated heat exchanger plates (30) in groups, the plate package (24) being comprised of heat exchanger plates (30) is packed in tower by top manhole, be embedded in beds (12), plate package (24) is whole to be supported jointly by being fixed on the annular gusset (34) of reactor shell (32) inwall and center discharge (5) outer wall;
Described heat exchanger plates (30) is quadrilateral structure, by two metallic plates, is welded, and all heat exchanger plates (30) in same reactor are identical;
The side that described metallic plate contacts with catalyst is parallel-plate fin structure, and plate wing (25) spacing is 0.1～0.5mm;
In the outer reaction zone of described beds (12), establish cold pipe (29);
The thickness of described heat exchanger plates (30) is 0.1～1.0mm;
Effective distance between plates of the interior adjacent heat exchanger plates of described beds (12) (30) or adjacent heat exchanger plates group (24) is 40～60mm;
Described outer distributing barrel (20), inside distributor (16) and gas redistributor (35) are cylindrical metal shell, on it, all establish perforate, press the flow direction of fluid, perforate distribution density in the upstream unit length that flows is larger, and the perforate distribution density in fluid flow downstream unit length is less.
2. plate-type reactor as claimed in claim 1, it is characterized in that, the arrangement mode of described plate package (24) in beds (12) is: be parallel to that beds (12) is radially placed and along concentric fan-shaped arranging, or perpendicular to beds (12), be radially similar to concentric circles and arrange.
3. plate-type reactor as claimed in claim 2, it is characterized in that, when plate package (24) is parallel to that beds (12) is radially placed and during along concentric fan-shaped arranging, according to the size of the size of reactor inner space and heat exchanger plates (30) itself, along same, radially establish a heat exchanger plates (30) or establish successively polylith heat exchanger plates (30); Apart from fixing by annular or circular fastening hoop (31) between the heat exchanger plates (30) of reactor axle center same distance.
4. plate-type reactor as claimed in claim 2, it is characterized in that, when plate package (24) is radially similar to concentric circles arrangement perpendicular to beds (12), same radially heat exchanger plates (30) is arranged in parallel, and the plate package (24) that is positioned at beds (12) is whole fixing by being positioned near outer distributing barrel (20) inwall and the outer peripheral circular fastening hoop of plate package (24) (31) encirclement.
5. plate-type reactor as claimed in claim 1, is characterized in that, two metallic plates of described heat exchanger plates (30) have identical impression, heat exchanger plates (30) hollow, two metallic plates weld along periphery, surperficial spot welding simultaneously, the formation fluid passage, gap between two metallic plates.
6. plate-type reactor claimed in claim 5, is characterized in that, described impression is corrugated, linear or bubbling shape.
7. plate-type reactor as claimed in claim 1, it is characterized in that, the fluid channel design of described plate type heat exchanging element, comprises successively along the flow direction of cooling medium: cooling medium inlet (7), main distributing pipe (22), plate package distributing pipe (23), plate package (24), heat exchanger plates steam outlet pipe (28), plate package steam collecting pipe (33), main collecting pipe (10) and steam outlet pipe mouth (9).
8. plate-type reactor as claimed in claim 1, is characterized in that, described cold pipe cross section (27) be shaped as triangle or parallelogram.
9. plate-type reactor as claimed in claim 8, it is characterized in that, when plate package (24) is parallel to that beds (12) is radially placed and during along concentric fan-shaped array, described cold pipe (29) is positioned between adjacent two heat exchanger plates (30) of outer reaction zone apart from reactor axle center same distance, is wedge shape and embeds in beds (12); When plate package (24) is radially similar to concentric circles arrangement perpendicular to beds, described cold pipe (29) is positioned between the adjacent heat exchanger plates group (24) of outer reaction zone apart from reactor axle center same distance.
10. plate-type reactor as claimed in claim 1, is characterized in that, the upper perforate of described inlet gas distributor (2) and exit gas distributor (13) is arranged as del or parallelogram.
11. plate-type reactors as claimed in claim 1, is characterized in that, the upper perforate of described inside distributor (16), outer distributing barrel (20) and gas redistributor (35) is circular, square, triangle, grid or fillet shape; Described perforate be arranged as circumferential or spirality.
12. plate-type reactors as described in as arbitrary in claim 1-11 are coupled the application in the technique of synthesis of oxalate technique or carbonylation coupled reaction synthesis of oxalic acid dialkyl and dialkyl carbonate at carbonylation.
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| CN104152170B (en) * | 2014-08-25 | 2015-12-09 | 安徽工程大学 | A kind of preparation method of diesel oil |
| CN105032305B (en) * | 2015-08-27 | 2017-10-20 | 德艾柯工程技术（上海）有限公司 | A kind of new radial direction plate-type reactor |
| CN106732311A (en) * | 2017-01-23 | 2017-05-31 | 南京敦先化工科技有限公司 | A kind of spherical cavity header coil pipe reactor of water route Natural Circulation |
| AR113649A1 (en) | 2017-12-20 | 2020-05-27 | Haldor Topsoe As | COOLED AXIAL FLOW CONVERTER |
| CN108745211B (en) * | 2018-08-08 | 2023-09-01 | 德艾柯工程技术（上海）有限公司 | Catalyst filling device of plate reactor |
| AU2018446829B2 (en) * | 2018-10-22 | 2022-12-15 | Pujing Chemical Industry Co., Ltd | Large-scale ethylene glycol reactor |
| CN115253924B (en) * | 2020-12-04 | 2023-06-16 | 中国成达工程有限公司 | Vertical radial flow reactor |
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| EP1221339A1 (en) * | 2001-01-05 | 2002-07-10 | Methanol Casale S.A. | Catalytic reactor with heat exchanger for exothermic and endothermic heterogeneous chemical reactions |
| CN2845904Y (en) * | 2004-12-14 | 2006-12-13 | 杭州林达化工技术工程有限公司 | Lateral tubular heat exchanging reaction device |
| EP1782883A1 (en) * | 2005-11-08 | 2007-05-09 | Methanol Casale S.A. | Isothermal chemical reactor |
| EP1854534A1 (en) * | 2006-05-12 | 2007-11-14 | Methanol Casale S.A. | Isothermal reactor |
| EP2070590A1 (en) * | 2007-12-11 | 2009-06-17 | Methanol Casale S.A. | Supporting system of heat-exchange plates in isothermal chemical reactors |
| CN201161185Y (en) * | 2008-03-07 | 2008-12-10 | 钱进华 | Double-layer heat exchange plate-type reactor in parallel |
| CN101462081A (en) * | 2008-10-25 | 2009-06-24 | 上海戊正工程技术有限公司 | Method for preparing catalyst for synthesizing dimethyl oxalate |
| CN102040474B (en) * | 2009-10-13 | 2013-07-31 | 中国石油化工股份有限公司 | Method for producing ethanediol from oxalic ester and hydrogen |
| CN202876772U (en) * | 2012-10-23 | 2013-04-17 | 上海戊正工程技术有限公司 | Industrialized plate type reactor for synthesizing ester by carbonylation coupling |
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