CN102872767A - 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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- CN102872767A CN102872767A CN201210407063XA CN201210407063A CN102872767A CN 102872767 A CN102872767 A CN 102872767A CN 201210407063X A CN201210407063X A CN 201210407063XA CN 201210407063 A CN201210407063 A CN 201210407063A CN 102872767 A CN102872767 A CN 102872767A
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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 ofly be coupled the industrialization plate-type reactor of 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 day by day minimizing of petroleum resources, preparing oxalate by the natural gas via synthesis gas is a ground-breaking C1 chemical industry new technology, new technology, realize with coal and substitute gas oil ethene, the strategic objective of indirect synthesizing glycol of two steps, have very large market prospects, particularly for the 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 carbonylation fixed bed reactors that are coupled synthesis of oxalate adopt shell and tube reactor substantially.Shell and tube reactor is made simple, but aspect the raising respond certain limitation is being arranged.Generally, improve respond and mainly solve by improving heat exchange area and loaded catalyst, namely will strengthen the quantity of diameter or the increase tubulation of tubulation.It is inhomogeneous to produce like this bed radial temperature profile, causes reacting wayward, and increases the generation of side reaction.In addition, when power requirement is high to a certain degree the time, the shell and tube reactor volume is larger, axially and radially larger temperature difference will cause the system capacity Efficiency Decreasing, even so that the hydrogenation reaction in the reactor can't normally 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 the optimum temperature curve.And present industrial employing shell and tube reactor is for avoiding the catalyst shortcomings such as aging, service life is short easily, usually 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 the catalyst bed layer height, thereby greatly increased equipment running resistance and power consumption.
In sum, present carbonylation is coupled the synthesis of oxalate reaction and has following shortcoming: the one, adopt the 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.Because the shortcoming of above two aspects, it is less to cause existing carbonylation to be coupled synthesis of oxalate inside reactor effective heat exchange area, and consumptive material is many, and equipment manufacturing cost is high, and bulky, and I﹠M is all inconvenient.In addition, because the shortcoming of above device structure, so that the average reaction temperature in the course of reaction is lower, it is low to cause carbonylation to be coupled the synthesis of oxalate reaction rate, and 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 resistance was little when a kind of gas flow was provided, power consumption is low, callable heat is many, output is high, production cost is low.It is low to solve and overcome the pipe type heat transfer heat transfer coefficient that the inner heat exchange structure of existing hydrogenation reactor exists, 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, the problem and the shortcoming that cause that hydrogenation reaction speed is low, the catalyst consumption are large, investment is large etc.Board-like gas-solid catalysis device provided by the invention, increased heat transfer coefficient in the chamber, therefore strengthened heat transfer, greatly reduced hot(test)-spot temperature, greatly increased the catalyst usage factor simultaneously, significantly reduced equipment running resistance and improved the production capacity of device.
The present invention realizes by the following technical solutions:
A kind ofly be coupled the industrialization plate-type reactor of synthesis of oxalate for carbonylation, 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; Establish the gas redistributor in the described beds, beds is divided into outer reaction zone and internal reaction district.
Establish heat exchanger in the described beds, 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 that is comprised of heat exchanger plates is packed into by the top manhole in the tower, be embedded in the beds, plate package integral body supports jointly by the annular gusset that is fixed on 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, perhaps radially be similar to concentric circles perpendicular to beds and arrange.The reaction medium of circulation between the various heat exchange plate has different cross-flow modes according to the different in kind of catalyst, and purpose is to prolong the circulation distance of reaction medium between plate, and guarantees that as far as possible each reaction medium circulation path pressure drop is near identical; Utilize arrange position or radially be similar to the concentric circles arrangement position perpendicular to beds of fan-shaped in reaction bed of plate type heat exchanger, can rationally utilize the inside reactor heat, realize preferably thermal coupling between vaporization and the reaction, increased heat-transfer effect, raising conversion ratio and purpose optionally thereby reach.
When plate package is radially placed and during along concentric fan-shaped arranging, according to the size of reactor inner space and the size of heat exchanger plates itself, radially can be established a heat exchanger plates or establish successively the 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 radially is similar to the 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 the flow through Area comparison of institute's contact catalyst of gas is large and evenly, the reaction combined coefficient is higher.Entire infrastructure all is the standard component of modular, in case 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, is welded by two metallic plates, and all heat exchanger plates in the 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, simultaneously surperficial spot welding, then punching press is made, and the slit between two metallic plates forms the fluid passage.When fluid flows through the plate of above-mentioned impression in the crankle mode, accelerated rate of flow of fluid on the one hand, greatly improved overall heat-transfer coefficient, and prolonged 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 simultaneously the plate inner fluid obtain preheating.
Described impression is corrugated, linear, polyline shaped or bubbling shape.
The side that described metallic plate contacts with catalyst is the parallel-plate fin structure, and plate wing spacing is 0.1～0.5mm; Adopt described parallel-plate fin structure, fluid is fully mixed in reaction zone improve heat transfer efficiency, overcome shell and tube reactor limitation in this respect, make simultaneously structure of reactor compacter, 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), and is 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: enter reactor from cooling medium inlet, enter in the heat exchanger plates of each plate package through main distributing pipe and plate package distributing pipe, after heat exchanger plates and beds heat exchange, produce and enter plate package steam collecting pipe after the low pressure saturated steam compiles in the heat exchanger plates steam outlet pipe, at last, discharge reactor through main collecting pipe from the steam outlet pipe mouth from the low pressure steam of plate package 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 in time shifted out beds, produces simultaneously low-pressure saturated steam; Also can gas-gas heat exchange.
The type of flow of the outer reactant of cooling medium and plate is cross-flow in the described heat exchanger plates.
Establish cold pipe in the outer reaction zone of described beds.
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 is wedge shape and embeds in the beds between adjacent two heat exchanger plates of distance reactor axle center same distance; Equate that with the effective distance between plates that keeps described adjacent two heat exchanger plates 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 radially is similar to the concentric circles arrangement perpendicular to beds, described cold pipe is between the adjacent heat exchanger plates group of distance reactor axle center same distance, being wedge shape embeds in the beds, equate that with effective distance between plates of keeping described adjacent two plate package the effective distance between plates between described adjacent plate package then deducts remaining distance behind the shared space of cold pipe for the distance between adjacent two plate package.
Effective distance between plates of adjacent heat exchanger plates or adjacent heat exchanger plates group is 40～60mm in the described beds, is preferably 40～50mm.
Medium in the 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 that flows 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, enters each cold pipe after cold pipe import distributing pipe distributes, and compiles cold pipe exit collector after cold pipe flows out, then outside 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 perforate is arranged and is inverted triangle or parallelogram on the distributor; Inverted triangle preferably.
Described outer distributing barrel, inside distributor and gas redistributor are the cylindrical metal shell, all establish perforate, press the flow direction of fluid, the perforate distribution density that is on the upstream unit length that flows is larger, and the perforate distribution density that is on the unit length of Fluid Flow in A downstream is less; Thereby guaranteed the even distribution of air-flow, reduce at the dead angle, has improved the utilization rate of catalyst.
Perforate on described outer distributing barrel, inside distributor and the gas redistributor is circular, square, triangle, grid or fillet shape; Be preferably fillet shape; Perforate is arranged as circumferential or spirality on the cylinder.
Described gas redistributor newly distributes for promoting the circulation of qi body weight that dissimilar catalyst are separately gone forward side by side.
The different catalyst of filling in described outer reaction zone and the internal reaction district, described outer reaction zone is away from the product equilibrium concentration, the reaction motive force is large, per volume of catalyst reaction liberated heat is many, therefore outer reaction zone is the reaction heat concentrated area that carbonylation is coupled the synthesis of oxalate reaction, and constantly carrying out along with oxonation in the internal reaction district, gas oxalate content is enrichment gradually, near the 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 in the inside and outside reaction zone is carried out different prioritization schemes with size, to strengthen the reaction diabatic process, make in the beds Temperature Distribution rationally and near the optimum temperature curve.
The particle size of the carbonylation catalyst of filling is 3.2～5.5 * 3.2～5.5mm in the described outer reaction zone, is preferably 5 * 5mm.
The shape of carbonylation catalyst comprises cylindrical, Raschig ring, clover, bunge bedstraw herb, the five fingers ball or sphere in the described outer reaction zone, is preferably Raschig ring.
Particle size 3.2～5.5 * 3.2～5.5mm of the catalyst of filling is preferably 3.2 * 3.2mm in the described internal reaction district.
The shape of carbonylation catalyst comprises cylindrical, Raschig ring, clover, bunge bedstraw herb, the five fingers ball or sphere in the described internal reaction district, is preferably the five fingers ball.
The carbonylation catalyst of described beds places in the space that reaches between heat exchanger plates and the heat exchanger plates between heat exchanger plates and the cold pipe.
The housing upper end of described plate-type reactor is provided with manhole, the lower end is established ring-shaped distributed catalyst and is drawn off the mouth of pipe, catalyst supports by lower end inert filler bed under the normal operating position, when drawing off catalyst, to draw off nozzle flange and lay down, the filler in the catalyst of catalytic bed and the 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 the preheating enters reactor by the Reactor inlet pipe, at first pass through the inlet gas distributor, then further preheating in Heat Room, again through the further uniform distribution of upper end inert filler layer, gas after the 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 the internal reaction district and continue reaction after redistributor distributes again; At last, most product enters the 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 the exit gas distributor simultaneously, flow out from the reactor outlet pipe.
Described plate-type reactor, be used for carbonylation and be coupled the 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 patent " a kind of technological process of producing ethylene glycol with coproduction product dimethyl carbonate " the ZL200810043079.0 claim, and such as the patent No. 201220194360.6, " a kind of acetate is produced the technique of ethanol and selective coproduction 2-butanols "; The acetate hydrogenation reactor of indication among the patent No. 201210134269.X " a kind of acetate is produced technique and the process matched therewith system thereof of ethanol and selective coproduction 2-butanols ".
The main feature of described plate-type reactor is that heat exchanger plates is inserted in the beds, leakes water in the plate or other heat transferring medium, and the heat exchange area of heat exchanger plates is larger than heat exchanger tube, so can take away more reaction heat.And the flow through Area comparison of institute's contact catalyst of gas is large and evenly, the reaction combined coefficient is higher.Entire infrastructure all is the standard component of modular, in case damage, can be easy to replace.Adopt the parallel fins plank frame, fluid fully mixes in fan-shaped reaction zone, overcomes shell and tube reactor limitation in this respect, the simultaneously raising of heat transfer efficiency, make structure of reactor compacter, less bed volume has been 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 the concentric circles distributing position, rationally utilize the inside reactor heat, realize preferably thermal coupling between vaporization and the reaction, increased heat-transfer effect, raising conversion ratio and purpose optionally thereby reach.
Described plate-type reactor fully excavates the potentiality of catalyst, greatly increased the catalyst usage factor, the equipment running resistance only is 1/6 of shell-and-tube reactor, the 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 having automatic mounting, unload the function of carried catalyst, start new way for current carbonylation is coupled the maximization of synthesis of oxalate reactor, had preferably promotion prospect and economic benefit.
Described plate-type reactor is used for carbonylation and is coupled the synthesis of oxalate industrialized unit, is convenient to the expansion scale.
Description of drawings
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 to be 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 for carbonylation that plate package radially is similar to concentric circles arrangement architecture schematic diagram perpendicular to beds in the industrialization plate-type reactor of synthesis of oxalate
Fig. 7 plate package radially is similar to concentric circles perpendicular to beds and arranges local structural graph
Fig. 8 plate package radially is 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 only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition 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 among the following embodiment, usually according to normal condition, such as the chemical industry operation handbook, or the condition of advising according to manufacturer.
The industrialization plate-type reactor (carrying out the 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 16 and 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; Establish gas redistributor 35 in the described beds 12, beds 12 is divided into outer reaction zone and internal reaction district.
12 establish heat exchanger in the described beds, 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 that is comprised of heat exchanger plates 30 is packed into by the top manhole in the tower, be embedded in the beds 12, plate package 24 integral body support jointly by the annular gusset 34 that is fixed on 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 all heat exchanger plates 30 are identical in the same reactor; Two metallic plates have identical bubbling shape impression, heat exchanger plates 30 hollows, and two metallic plates weld along periphery, simultaneously surperficial spot welding, then punching press is made, and the slit between two metallic plates forms the fluid passage; The side that metallic plate contacts with catalyst is the parallel-plate fin structure, and plate wing 25 spacings 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; Radially establish 3 heat exchanger plates 30 along same; 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.
Along the outer reaction zone of described beds 12 away from establishing cold pipe 29 between two adjacent heat exchanger plates 30 of discharge 5 places in center 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, namely guarantee catalyst radially tangent plane filling overall width be 40mm.Filling is used for the catalyst that carbonylation is coupled synthesis of oxalate between the heat exchanger plates 30 of beds 12 and heat exchanger plates 20 and in the space between heat exchanger plates 30 and the cold pipe 29.During reaction, logical supercooling tube 29 is taken away unnecessary beds 12 heat of reaction by indirect heat exchange, to guarantee that outer reaction zone beds 12 Temperature Distribution are as the optimal temperature distribution.
The channels designs of described cold pipe 29, the direction that flows 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, perforate is arranged as del on the distributor.
Described outer distributing barrel 20, inside distributor 16 and gas redistributor 35 are the 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 that is on the unit length of Fluid Flow in A upstream is larger, and the perforate distribution density that is on the unit length of Fluid Flow in A downstream is less, thereby has guaranteed the even distribution of air-flow, reduce at the 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 the internal reaction district; The carbonylation catalyst of filling is shaped as Raschig ring in the described outer reaction zone, and particle size is 5 * 5mm; In the described internal reaction district 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 in the form of a ring, and the catalyst of apportion draws off the mouth of pipe 8, catalyst supports by reactor lower end inert filler layer 6 under the normal operating position, when drawing off catalyst, catalyst is drawn off the mouth of pipe 8 flanges 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.
Walk boiler feedwater (CL in the heat exchanger plates 30
-Less than 4PPM), enter reactor from cooling medium inlet 7, enter in each plate package 24 through main distributing pipe 22, then behind plate package distributing pipe 23, enter in the heat exchanger plates 30 of each plate package 24, behind heat exchanger plates 30 and catalyst heat exchange, produce and enter plate package steam collecting pipe 33 after the low pressure saturated steam compiles in heat exchanger plates steam outlet pipe 28, at last, discharge reactor through main collecting pipe 10 from steam outlet pipe mouth 9 from the low pressure steam of plate package 24 and deliver to extraneous the recycling, sending water vapour pressure outside is 0.3～0.5MPa.
Also walk boiler feedwater in the cold pipe 29, 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 compiling, cold pipe exit collector 19 discharges reactor from cold pipe outlet 18, logical like this supercooling tube 29 auxiliary heat-exchangings are to guarantee that outer reaction zone beds 12 Temperature Distribution are as the optimal temperature distribution, thereby guarantee that the high conversion of catalyst with selective, improves the catalyst usage factor.
When carrying out the carbonylation coupled reaction, mist (105 ℃ of temperature, pressure 0.2MPa) enters upper end inert filler layer 3 from cat head Reactor inlet pipe 1 by inlet gas distributor 2 first, to strengthen distribution of gas, Heat Room 15 interior through further with the steam indirect heat exchange after and after the gas phase redistribution, mixing temperature reaches 140 ℃, flow down along reactor shell 32 inwalls and 20 annular spaces 11 of outer distributing barrel, enter the outer reaction zone of beds 12 by the outer distributing barrel 20 of reaction bed 4 radially, outer reaction zone beds 12 temperature are controlled at 120～130 ℃, reaction conversion ratio 50%, dimethyl oxalate selective 70%; Reaction heat has been avoided the accumulation of heat, thereby has been guaranteed that reaction bed does not become high focus owing to shifts out rapidly under the catalyst shape acting in conjunction of good plate heat transfer efficiency and larger catalyst granules and hollow.Then the internal reaction district that together enters beds 12 after reacting gas and reaction product gas redistribute through redistributor 35 continues reaction, and internal reaction district temperature is controlled at 130～140 ℃, reaction conversion ratio 85%, dimethyl oxalate selective 94%.This moment, qualified thick oxalate was produced in reaction, and it is 135 ℃ that material goes out temperature of reactor.At last, 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, flow out from reactor outlet pipe 14, reaction bed pressure is reduced to 0.06MPa.
Described plate-type reactor can obtain more massive reaction unit by the size that increases the unit process body or the quantity that increases the unit process body.This just is different from the too huge shortcoming of volume after the shell and tube reactor expansion scale.
Claims (19)
1. one kind is used for the industrialization plate-type reactor that carbonylation is coupled synthetic ester, 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; Establish gas redistributor (35) in the described beds (12), beds (12) is divided into outer reaction zone and internal reaction district.
2. plate-type reactor as claimed in claim 1 is characterized in that, 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) that is comprised of heat exchanger plates (30) is packed into by the top manhole in the tower, be embedded in the beds (12), plate package (24) is whole to be supported by the annular gusset (34) that is fixed on reactor shell (32) inwall and center discharge (5) outer wall is common.
3. plate-type reactor as claimed in claim 2, 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, perhaps radially be similar to concentric circles perpendicular to beds (12) and arrange.
4. plate-type reactor as claimed in claim 3, 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 reactor inner space and the size of heat exchanger plates (30) itself, radially establish a heat exchanger plates (30) or establish successively polylith heat exchanger plates (30) along same; Apart from fixing by annular or circular fastening hoop (31) between the heat exchanger plates (30) of reactor axle center same distance.
5. plate-type reactor as claimed in claim 3, it is characterized in that, when plate package (24) radially is similar to the 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.
6. plate-type reactor according to claim 2 is characterized in that, the thickness of described heat exchanger plates (30) is 0.1～1.0mm.
7. plate-type reactor as claimed in claim 2 is characterized in that, described heat exchanger plates (30) is quadrilateral structure, is welded by two metallic plates, and all heat exchanger plates (30) in the same reactor are identical.
8. plate-type reactor as claimed in claim 7 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, simultaneously surperficial spot welding, and the slit between two metallic plates forms the fluid passage.
9. plate-type reactor claimed in claim 8 is characterized in that, described impression is corrugated, linear, polyline shaped or bubbling shape.
10. such as the arbitrary described plate-type reactor of claim 7-9, it is characterized in that the side that described metallic plate contacts with catalyst is the parallel-plate fin structure, plate wing (25) spacing is 0.1～0.5mm.
11. plate-type reactor as claimed in claim 2, 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).
12. require 1 described plate-type reactor such as profit, it is characterized in that, establish cold pipe (29) in the outer reaction zone of described beds (12).
13. plate-type reactor as claimed in claim 12 is characterized in that, described cold pipe cross section (27) be shaped as triangle, square, rhombus or parallelogram.
14. plate-type reactor as claimed in claim 12, 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 the beds (12); When plate package (24) radially was similar to the concentric circles arrangement perpendicular to beds, described cold pipe (29) was positioned between the adjacent heat exchanger plates group (24) of outer reaction zone apart from reactor axle center same distance.
15. plate-type reactor as claimed in claim 14 is characterized in that, 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.
16. 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.
17. plate-type reactor as claimed in claim 1, it is characterized in that, described outer distributing barrel (20), inside distributor (16) and gas redistributor (35) are the cylindrical metal shell, all establish perforate on it, press the flow direction of fluid, the perforate distribution density that is on the upstream unit length that flows is larger, and the perforate distribution density that is on the unit length of Fluid Flow in A downstream is less.
18. plate-type reactor as claimed in claim 17 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.
19. be coupled application in the technique of synthesis of oxalate technique or carbonylation coupled reaction synthesis of oxalic acid dialkyl and dialkyl carbonate such as the arbitrary described plate-type reactor of claim 1-18 at carbonylation.
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