CN112588208A - Process for preparing ethyl lactate by catalytic esterification of fixed bed reactor - Google Patents
Process for preparing ethyl lactate by catalytic esterification of fixed bed reactor Download PDFInfo
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- CN112588208A CN112588208A CN202011527800.0A CN202011527800A CN112588208A CN 112588208 A CN112588208 A CN 112588208A CN 202011527800 A CN202011527800 A CN 202011527800A CN 112588208 A CN112588208 A CN 112588208A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
- B01J8/065—Feeding reactive fluids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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Abstract
The invention relates to a process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor, which comprises the following steps: step A: inputting a mixed material of lactic acid and ethanol into the fixed bed reactor from a feed inlet of the fixed bed reactor; and B: the material entering the fixed bed reactor is input into the tube nest of the fixed bed reactor through the material distribution disc of the fixed bed reactor; and C: reacting the materials in a tube; step D: and the reacted materials are discharged from the tube array and then are collected at the bottom of the fixed bed reactor, and are discharged from a discharge hole of the fixed bed reactor. In the invention, the supporting component is arranged and consists of a plurality of connecting components, so that the tubes can be conveniently fixed and supported, and the width of the clamping plate can be set according to requirements, so that the contact part of the clamping plate and the tubes has a larger contact area, and the tubes can be effectively prevented from being abraded, fatigue of materials and the like when the tubes vibrate, thereby reducing the leakage probability of the tubes.
Description
Technical Field
The invention relates to the technical field of fixed bed reactors. In particular to a process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor.
Background
In the process of preparing ethyl lactate by catalytic esterification, a fixed bed reactor is needed, the traditional fixed bed reactor adopts a feeding mode of feeding from bottom to top, and has the problems of bias flow, material back mixing and the like, when the fixed bed reactor is used, a tube array can vibrate due to various factors, the contact area between a tube plate used for supporting and fixing the middle part of the tube array and the tube array is smaller, after the tube array vibrates for a long time, the contact part of the tube array and the tube plate is fatigue, cracks are generated to cause tube array abrasion, and leakage is caused, the traditional tube plate is of an integral plate-shaped structure, the flow of heat exchange liquid in a shell pass can be influenced, the heat conductivity of the traditional fixed bed reactor is poorer, the heat exchange efficiency is further influenced, and the inside and the outside of the tube plate have larger temperature difference, so that the temperature difference stress is larger; the bottom of the existing tube nest has certain inconvenience when supporting the catalyst, and certain troubles exist in disassembly and assembly.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor, which improves the heat exchange efficiency, reduces the temperature difference stress on two sides of a tube plate and is convenient for supporting a catalyst.
In order to solve the technical problems, the invention provides the following technical scheme: the process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor comprises the following steps:
step A: inputting a mixed material of lactic acid and ethanol into the fixed bed reactor from a feed inlet of the fixed bed reactor;
and B: the material entering the fixed bed reactor is input into the tube nest of the fixed bed reactor through the material distribution disc of the fixed bed reactor;
and C: reacting the materials in a tube;
step D: and the reacted materials are discharged from the tube array and then are collected at the bottom of the fixed bed reactor, and are discharged from a discharge hole of the fixed bed reactor.
The fixed bed reactor further comprises a tank body, an upper tube plate and a lower tube plate which are respectively arranged at two ends of the inner wall of the tank body, an upper end socket and a lower end socket which are respectively fixedly connected with two ends of the tank body, and a tube nest which is positioned in the tank body and is respectively connected with the upper tube plate and the lower tube plate at two ends, wherein an auxiliary heat exchange assembly is arranged between the upper tube plate and the lower tube plate, a catalyst supporting assembly is arranged in the lower end of the tube nest, a supporting assembly is arranged in the middle of the tube nest, and the side wall of the supporting assembly is fixedly connected with the side face of the inner wall of the tank body.
According to the process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor, the supporting assembly comprises a supporting ring and a plurality of connecting assemblies, and the four connecting assemblies are arranged on the side surface of the tube array along the circumferential direction of the tube array; the connecting assembly comprises a first fixing frame in the middle, the first fixing frame is cross-shaped, four end parts of the first fixing frame are provided with sockets, connecting rods are inserted in the sockets, a clamping plate is arranged at the second end of each connecting rod, the side wall of each clamping plate is fixedly connected with a connecting seat, the connecting seats are fixedly connected with the second end of each connecting rod, heat exchange plates are fixedly connected to two sides of each connecting seat, the clamping plates are quarter-ring-shaped, and two ends of each connecting rod are fixedly connected with the connecting seats and the end parts of the first fixing frame respectively through bolts; the connecting component close to the inner side wall of the support ring is fixedly connected with the inner wall of the support ring through a connecting rod, and the outer side wall of the support ring is fixedly connected with the inner wall of the tank body.
In the process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor, the catalyst supporting component is used for wrapping the fixed rod, the first end of the fixed rod is movably connected with the first fixed sleeve, the first end part of the fixed rod is fixedly connected with the fixed plate, the second end of the fixed rod is sleeved with the second fixed sleeve, the end part of the first fixed sleeve is provided with the metal net, the inner side of the metal net is sleeved at the first end of the fixed rod, the side wall of the fixed plate is lapped with the side wall of the metal net, the side wall of the first fixed sleeve is hinged with the supporting rod through a pin shaft, the second end of the supporting rod is hinged with the pressing plate, the outer side of the metal net is lapped with the side wall of the pressing plate, the side face of the second fixed sleeve is hinged with the hinged rod, the second end of the hinged rod is hinged, the top of the nut is lapped with the bottom of the second fixing sleeve, and the surface of the metal net is a conical surface; the number of the support rods, the number of the hinge rods and the number of the pressing plates are three or more, the side walls of the pressing plates are in lap joint with the side faces of the inner walls of the tubes, and the edges of the metal nets are tightly pressed in the tubes.
In the process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor, the auxiliary heat exchange assembly comprises a first liquid distribution ring, a second liquid distribution ring and a third liquid distribution ring, the first liquid distribution ring, the second liquid distribution ring and the third liquid distribution ring are all in a circular ring shape, the outer diameters of the first liquid distribution ring, the second liquid distribution ring and the third liquid distribution ring are sequentially reduced, the first liquid distribution ring, the second liquid distribution ring and the third liquid distribution ring are all fixedly connected with the side surface of the inner wall of the tank body through a second fixing frame, the outer side walls of the first liquid distribution ring, the second liquid distribution ring and the third liquid distribution ring are all communicated with liquid supply pipes, the liquid supply pipes penetrate through the side wall of the tank body, the end parts of the three liquid supply pipes are communicated with a distribution pipe, the middle parts of the distribution pipes are communicated with liquid inlet pipes, and the tops of the first liquid distribution ring, the second liquid distribution ring and the third liquid distribution ring are respectively communicated with, a plurality of through holes are uniformly formed in the side wall of the vertical pipe along the circumferential direction and the axial direction of the vertical pipe; the first liquid distribution ring, the second liquid distribution ring and the third liquid distribution ring are coaxially arranged and are positioned above the lower tube plate and close to the lower tube plate.
According to the process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor, the side face of the inner wall side of the upper end enclosure is fixedly connected with the two material distribution discs, the material distribution discs are conical, and the top of each material distribution disc is uniformly provided with the material inlet holes.
According to the process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor, the bottom of the lower end enclosure is communicated with the discharge hole, the top of the upper end enclosure is communicated with the feed hole, the lower part of the side surface of the tank body is communicated with the three liquid inlet pipes, the three liquid inlet pipes are uniformly distributed along the circumferential direction of the tank body, and the top of the side surface of the tank body is communicated with the liquid outlet pipe.
According to the process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor, the side wall of the upper tube plate is fixedly connected with the top of the inner wall of the tank body, the side wall of the lower tube plate is fixedly connected with the bottom of the inner wall of the tank body, and two ends of the tube array penetrate through the upper tube plate and the lower tube plate respectively and are fixedly connected with the upper tube plate and the lower tube plate respectively.
According to the process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor, the top of the upper tube plate and the bottom of the lower tube plate are both provided with the coil pipes, the bottom of the coil pipe at the top of the upper tube plate is tightly attached to the top of the upper tube plate, one end of the coil pipe at the top of the upper tube plate penetrates through the middle of the upper tube plate, the other end of the coil pipe penetrates out of the tank body, the top of the coil pipe at the bottom of the lower tube plate is tightly attached to the bottom of the lower tube plate, one end of the coil pipe at the bottom of the lower tube plate.
In the process for preparing the ethyl lactate by using the fixed bed reactor for catalytic esterification, the inner side wall of the tank body and the side surfaces of the tubes are provided with a plurality of baffle plates; and the vertical pipes of the auxiliary heat exchange assemblies penetrate between the tubes.
The technical scheme of the invention achieves the following beneficial technical effects:
1. according to the invention, by arranging the supporting component, the supporting component is composed of a plurality of connecting components, so that the tubes can be conveniently fixed and supported, and because the width of the clamping plate can be set according to requirements, compared with the traditional tube plate type fixing method, the clamping plate has a larger contact area with the contact part of the tubes, so that when the tubes vibrate, the tubes can be effectively prevented from being abraded, the material is fatigue and the like, and the leakage probability of the tubes is reduced; after the tubes are supported by the plurality of supporting assemblies, the heat exchange liquid can directly flow through gaps among the plurality of supporting assemblies, so that the transverse flow of the heat exchange liquid can be reduced, the vibration of the pipeline caused by the transverse flow of the heat exchange liquid is reduced, and when the heat exchange liquid flows through the heat exchange plate, the heat exchange plate and the tubes exchange heat, so that the heat exchange area is further increased; compare in supporting through the tube sheet through the mode that a plurality of supporting components fixed and supported the tubulation, because tube sheet formula as an organic whole, it is bigger that it receives expend with heat and contract with cold's influence, when the tube sheet inflation, can exert pressure to the tube wall, bring certain adverse effect, and supporting component has a plurality of part equipment to form, there is certain fit clearance between part and the part, a plurality of supporting component cooperations back, when it takes place expend with heat and contract with cold, the size variation of each part can carry out the part through the fit clearance between the part and offset, reduce its influence that receives expend with heat and contract with cold, thereby reduce the pressure applying to the jar body.
2. According to the invention, the auxiliary heat exchange assemblies are arranged, so that heat exchange can be respectively conducted to the liquid dividing rings, liquid is conducted to the vertical pipes by the liquid dividing rings and discharged, the vertical pipes are arranged between the tubular columns in a penetrating mode, heat exchange liquid can be directly filled between the tubular columns, and the heat exchange liquid is diffused outwards from the vertical pipes, so that heat exchange dead zones are reduced, and heat exchange efficiency is improved.
3. According to the catalyst support assembly, the catalyst support assembly can be conveniently placed at the bottom of the tube nest and supports the catalyst, the support can be realized only by screwing the nut during placement, and the conical metal net has a larger surface area than a circular metal net, so that the resistance to reactants can be reduced; through setting up the coil pipe, the one end and the heat transfer liquid intercommunication of its coil pipe, when carrying out the heat transfer in the shell side, the heat transfer liquid can be in the same direction as the coil pipe and flow, and the tube sheet is hugged closely to the coil pipe to heat the outside of tube sheet, avoid the inside and outside difference in temperature of tube sheet too big, in order to reduce the influence of difference in temperature stress to last tube sheet and lower tube sheet.
Drawings
FIG. 1 is a schematic front sectional view of the present invention;
FIG. 2 is a schematic top view of the support assembly of the present invention;
FIG. 3 is a schematic perspective view of a connecting assembly of the present invention;
FIG. 4 is a schematic view of a plurality of connecting members of the present invention after they are connected;
FIG. 5 is a schematic top view of an auxiliary heat exchange assembly according to the present invention;
FIG. 6 is a schematic view of the cross-sectional front view of the auxiliary heat exchange assembly of the present invention;
FIG. 7 is an enlarged view of FIG. 6A of the present invention;
FIG. 8 is a schematic top view of the coil of the present invention;
FIG. 9 is a schematic diagram of a front cross-sectional view of a catalyst support assembly according to the present invention.
The reference numbers in the figures denote: 1-tank body; 2-lower end enclosure; 3, sealing the head; 4-an upper tube plate; 5-lower tube plate; 6-liquid inlet pipe; 7-a liquid outlet pipe; 8-a discharge hole; 9-a feed inlet; 10-a support assembly; 101-a support ring; 102-a connection assembly; 103-a first mount; 104-a connecting rod; 105-a splint; 106-heat exchange plates; 107-a connecting seat; 11-a baffle plate; 12-tube array; 13-an auxiliary heat exchange assembly; 14-a catalyst support assembly; 141-a fixing rod; 142-a first fixation sleeve; 143-fixing plate; 144-a support bar; 145-metal mesh; 146-a platen; 147-a hinge rod; 148-a second fixation sleeve; 149-nut; 15-a coil pipe; 16-a first liquid separation ring; 17-a second liquid separation ring; 18-third hydroextraction ring; 19-a second mount; 20-a supply tube; 21-a distribution pipe; 22-a liquid inlet pipe; 23-a standpipe; 24-a via hole; 25-material distribution disc.
Detailed Description
The process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor comprises the following steps:
step A: inputting materials into the fixed bed reactor from a feed inlet 9 of the fixed bed reactor;
and B: the materials entering the fixed bed reactor are input into the tube nest 12 of the fixed bed reactor through the material distribution disc 25 of the fixed bed reactor;
and C: the materials react in the tube 12;
step D: the reacted materials are discharged from the tube array 12, collected at the bottom of the fixed bed reactor and discharged from the discharge port 8 of the fixed bed reactor.
Referring to fig. 1, the fixed bed reactor further includes a tank body 1, an upper tube plate 4 and a lower tube plate 5 respectively disposed at two ends of an inner wall of the tank body 1, an upper head 3 and a lower head 2 respectively fixedly connected to two ends of the tank body 1, and a tube array 12 located inside the tank body 1 and having two ends respectively connected to the upper tube plate 4 and the lower tube plate 5, wherein two material distribution discs 25 are fixedly connected to a side surface of the inner wall of the upper head 3, the material distribution discs 25 are tapered, material inlet holes are uniformly formed at tops of the material distribution discs 25, a material outlet 8 is communicated with a bottom of the lower head 2, a material inlet 9 is communicated with a top of the upper head 3, three liquid inlet tubes 6 are communicated with a lower portion of the side surface of the tank body 1, the three liquid inlet tubes 6 are uniformly distributed along a circumferential direction of the tank body 1, a liquid outlet tube 7 is communicated with a top of the side surface of the tank body 1, a, the side wall of the lower tube plate 5 is fixedly connected with the bottom of the inner wall of the tank body 1, and two ends of the tube array 12 respectively penetrate through the upper tube plate 4 and the lower tube plate 5 and are respectively fixedly connected with the upper tube plate 4 and the lower tube plate 5.
An auxiliary heat exchange assembly 13 is arranged between the upper tube plate 4 and the lower tube plate 5, as shown in fig. 5-7, the auxiliary heat exchange assembly 13 includes a first liquid distribution ring 16, a second liquid distribution ring 17 and a third liquid distribution ring 18, the first liquid distribution ring 16, the second liquid distribution ring 17 and the third liquid distribution ring 18 are all in a circular ring shape, the outer diameters of the first liquid distribution ring 16, the second liquid distribution ring 17 and the third liquid distribution ring 18 are sequentially reduced, the first liquid distribution ring 16, the second liquid distribution ring 17 and the third liquid distribution ring 18 are all fixedly connected with the side surface of the inner wall of the tank body 1 through a second fixing frame 19, the outer side walls of the first liquid distribution ring 16, the second liquid distribution ring 17 and the third liquid distribution ring 18 are all communicated with liquid supply tubes 20, the liquid supply tubes 20 penetrate through the side wall of the tank body 1, the end portions of the three liquid supply tubes 20 are communicated with a distribution tube 21, the middle portion of the liquid supply tube 21 is communicated with a, the top parts of the first liquid dividing ring 16, the second liquid dividing ring 17 and the third liquid dividing ring 18 are respectively communicated with a vertical pipe 23 along the circumferential direction, and the side wall of the vertical pipe 23 is uniformly provided with a plurality of through holes 24 along the circumferential direction and the axial direction; first branch liquid ring 16, second branch liquid ring 17 and third branch liquid ring 18 coaxial setting just are located the top of tube sheet 5 down and are close to tube sheet 5 down, the inside catalyst supporting component 14 that is provided with of lower extreme of tubulation 12 through setting up supplementary heat exchange assemblies 13, can let in the branch liquid ring respectively with the heat transfer, divides the liquid ring to let in standpipe 23 with liquid and discharge, because standpipe 23 wears to establish between tubulation 12, can directly fill heat-transfer liquid into between tubulation 12, from standpipe 23 outdiffusion heat-transfer liquid to reduce the heat transfer blind spot, improve heat exchange efficiency.
A support assembly 10 is arranged in the middle of the tube array 12, as shown in fig. 2-4, the support assembly 10 comprises a support ring 101 and a plurality of connecting assemblies 102, and the four connecting assemblies 102 are arranged on the side surfaces of the tube array 12 along the circumferential direction of the tube array 12; the connecting assembly 102 comprises a first fixing frame 103 in the middle, the first fixing frame 103 is cross-shaped, four end portions of the first fixing frame 103 are provided with sockets, a connecting rod 104 is inserted in each socket, a clamping plate 105 is arranged at the second end of the connecting rod 104, a connecting seat 107 is fixedly connected to the side wall of the clamping plate 105, the connecting seat 107 is fixedly connected with the second end of the connecting rod 104, heat exchange plates 106 are fixedly connected to two sides of the connecting seat 107, the clamping plate 105 is quarter-ring-shaped, and two ends of the connecting rod 104 are fixedly connected with the connecting seat 107 and the end portion of the first fixing frame 103 through bolts; the connecting component 102 close to the inner side wall of the support ring 101 is fixedly connected with the inner wall of the support ring 101 through the connecting rod 104, the outer side wall of the support ring 101 is fixedly connected with the inner wall of the tank body 1, the support component 10 is arranged, the support component 10 is composed of the connecting components 102, the tubular column 12 can be conveniently fixed and supported, and the width of the clamping plate 105 can be set according to requirements, compared with the traditional tubular plate type fixing method, the contact part of the tubular column 12 has a larger contact area, so that when the tubular column 12 vibrates, the tubular column 12 can be effectively prevented from being worn, the material fatigue and the like, the probability of leakage of the tubular column 12 is reduced, after the tubular column 12 is supported by the supporting components 10, the gaps among the supporting components 10 can enable heat exchange liquid to directly flow through, the cross flow of the heat exchange liquid can be reduced, and the pipeline vibration caused by the cross flow of the heat exchange liquid is, when the heat exchange liquid flows through the heat exchange plates 106, the heat exchange liquid exchanges heat with the tube nest 12 through the heat exchange plates 106, and the heat exchange area is further increased; compared with the mode of supporting the tubes 12 by the tube plates, the mode of fixing and supporting the tubes 12 by the support assemblies 10 is that the tube plates are integrated, and the tube plates are greatly affected by expansion with heat and contraction with cold, when the tube plates expand, pressure is applied to the tube walls to bring certain adverse effect, the support assemblies 10 are formed by assembling a plurality of parts, certain fit gaps exist among the parts, after the support assemblies 10 are matched, the size change quantity of each part can be partially offset through the fit gaps among the parts when the support assemblies expand with heat and contract with cold, and the influence of expansion with heat and contraction with cold is reduced, so that the pressure applied to the tank body 1 is reduced, as shown in fig. 9, the side walls of the support assemblies 10 are fixedly connected with the side surfaces of the inner walls of the tank body 1, the catalyst support assemblies 14 wrap fixing rods 141, first ends of the fixing rods 141 are movably connected with first fixing sleeves 142, and first end parts of the fixing rods 141 are fixedly connected, a second fixing sleeve 148 is sleeved at a second end of the fixing rod 141, a metal mesh 145 is arranged at the end of the first fixing sleeve 142, the inner side of the metal mesh 145 is sleeved at the first end of the fixing rod 141, the side wall of the fixing plate 143 is overlapped with the side wall of the metal mesh 145, the side wall of the first fixing sleeve 142 is hinged with a support rod 144 through a pin shaft, the second end of the support rod 144 is hinged with a press plate 146, the outer side of the metal mesh 145 is overlapped with the side wall of the press plate 146, the side surface of the second fixing sleeve 148 is hinged with a hinge rod 147, the second end of the hinge rod 147 is hinged with the middle part of the support rod 144, external threads are arranged on the surface of the fixing rod 141, a nut 149 is in threaded connection with the surface of the fixing rod 141, the top of the nut 149 is overlapped with the bottom; the number of the support rods 144, the number of the hinge rods 147 and the number of the pressure plates 146 are three or more, the side walls of the pressure plates 146 are lapped with the side surfaces of the inner walls of the tubes 12, the edges of the metal nets 145 are tightly pressed in the tubes 12, the catalyst support assembly 14 can be conveniently placed at the bottom of the tubes 12 to support the catalyst, when the catalyst support assembly is placed, the support can be realized only by screwing the nuts 149, and the conical metal nets 145 have larger surface area compared with the circular metal nets 145, so that the resistance to reactants can be reduced; through setting up coil pipe 15, its coil pipe 15's one end and heat transfer liquid intercommunication, when carrying out the heat transfer in the shell side, heat transfer liquid can be in the same direction as coil pipe 15 and flow, and the tube sheet is hugged closely to coil pipe 15 to heat the outside of tube sheet, avoid the inside and outside difference in temperature of tube sheet too big, in order to reduce the influence of difference in temperature stress to going up tube sheet 4 and tube sheet 5 down.
The working process is as follows: when the device is used, after a catalyst is filled into the tubes 12, the catalyst support assembly 14 is inserted into the bottom of the tubes 12, the nut 149 is screwed to push the second fixed sleeve 148 upwards, the second fixed push the hinge rod 147 and drive the support rod 144 to expand, the press plate 146 is pressed against the inner wall of the tubes 12, so as to support and fix the metal mesh 145, and play a role in supporting the catalyst, the liquid supply pipe 20 and the liquid inlet pipe 6 are both communicated with a circulating pump for shell-side heat exchange, so that heat exchange liquid enters the shell-side and auxiliary heat exchange assemblies 13, the heat exchange liquid enters the auxiliary heat exchange assemblies 13, then respectively enters the first liquid distribution ring 16, the second liquid distribution ring 17 and the third liquid distribution ring 18, then enters each vertical pipe 23, and flows out through the through holes 24 on the side surfaces of the vertical pipes 23, the flow speed of the heat exchange liquid between the tubes 12 is improved, heat exchange dead zones are reduced, and reaction raw materials enter through the feed inlet 9, and enters the tube pass after passing through the two material distribution discs 25 to react with the catalyst, and finally converges into the lower end enclosure 2 and flows out of the discharge hole 8.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications are possible which remain within the scope of the appended claims.
Claims (10)
1. The process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor is characterized by comprising the following steps:
step A: inputting a mixed material of lactic acid and ethanol into the fixed bed reactor from a feed inlet (9) of the fixed bed reactor;
and B: the material entering the fixed bed reactor is input into a tube nest (12) of the fixed bed reactor through a material distribution disc (25) of the fixed bed reactor;
and C: the materials react in the tube nest (12);
step D: the reacted materials are discharged from the tube array (12), collected at the bottom of the fixed bed reactor and discharged from a discharge hole (8) of the fixed bed reactor.
2. The process for preparing ethyl lactate by catalytic esterification according to claim 1, it is characterized in that the fixed bed reactor also comprises a tank body (1), an upper tube plate (4) and a lower tube plate (5) which are respectively arranged at the two ends of the inner wall of the tank body (1), an upper seal head (3) and a lower seal head (2) which are respectively and fixedly connected with the two ends of the tank body (1), and a tube nest (12) which is positioned in the tank body (1) and is respectively connected with the upper tube plate (4) and the lower tube plate (5) at the two ends, an auxiliary heat exchange assembly (13) is arranged between the upper tube plate (4) and the lower tube plate (5), a catalyst supporting component (14) is arranged in the lower end of the tube array (12), the middle part of the tube nest (12) is provided with a supporting component (10), and the side wall of the supporting component (10) is fixedly connected with the side surface of the inner wall of the tank body (1).
3. The process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor according to claim 2, wherein the supporting assembly (10) comprises a supporting ring (101) and a plurality of connecting assemblies (102), and the four connecting assemblies (102) are arranged on the side surfaces of the tubes (12) along the circumferential direction of the tubes (12); the connecting assembly (102) comprises a first fixing frame (103) in the middle, the first fixing frame (103) is cross-shaped, four end parts of the first fixing frame (103) are provided with sockets, connecting rods (104) are inserted in the sockets, a clamping plate (105) is arranged at the second end of each connecting rod (104), the side wall of each clamping plate (105) is fixedly connected with a connecting seat (107), each connecting seat (107) is fixedly connected with the second end of each connecting rod (104), heat exchange plates (106) are fixedly connected to two sides of each connecting seat (107), the clamping plate (105) is quarter-ring-shaped, and two ends of each connecting rod (104) are fixedly connected with the end parts of each connecting seat (107) and the first fixing frame (103) respectively through bolts; the connecting component (102) close to the inner side wall of the support ring (101) is fixedly connected with the inner wall of the support ring (101) through a connecting rod (104), and the outer side wall of the support ring (101) is fixedly connected with the inner wall of the tank body (1).
4. The process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor according to claim 2, wherein the catalyst support assembly (14) comprises a fixing rod (141), a first fixing sleeve (142) is movably connected to a first end of the fixing rod (141), a fixing plate (143) is fixedly connected to a first end of the fixing rod (141), a second fixing sleeve (148) is sleeved on a second end of the fixing rod (141), a metal mesh (145) is arranged at an end of the first fixing sleeve (142), an inner side of the metal mesh (145) is sleeved on the first end of the fixing rod (141), a side wall of the fixing plate (143) is overlapped with a side wall of the metal mesh (145), a support rod (144) is hinged to a side wall of the first fixing sleeve (142) through a pin shaft, a pressing plate (146) is hinged to a second end of the support rod (144), and an outer side of the metal mesh (145) is overlapped with a side wall of the pressing plate (, the side surface of the second fixing sleeve (148) is hinged with a hinge rod (147), the second end of the hinge rod (147) is hinged with the middle part of the support rod (144), the surface of the fixing rod (141) is provided with external threads, the surface of the fixing rod (141) is in threaded connection with a nut (149), the top of the nut (149) is overlapped with the bottom of the second fixing sleeve (148), and the surface of the metal mesh (145) is a conical surface; the number of the support rods (144), the number of the hinge rods (147) and the number of the pressing plates (146) are three or more, the side walls of the pressing plates (146) are in lap joint with the side faces of the inner walls of the tubes (12), and the edges of the metal nets (145) are pressed in the tubes (12).
5. The process for preparing ethyl lactate by catalytic esterification of a fixed bed reactor according to claim 2, wherein the auxiliary heat exchange assembly (13) comprises a first liquid distribution ring (16), a second liquid distribution ring (17) and a third liquid distribution ring (18), the first liquid distribution ring (16), the second liquid distribution ring (17) and the third liquid distribution ring (18) are all circular rings, the outer diameters of the first liquid distribution ring (16), the second liquid distribution ring (17) and the third liquid distribution ring (18) are sequentially reduced, the first liquid distribution ring (16), the second liquid distribution ring (17) and the third liquid distribution ring (18) are all fixedly connected with the side surface of the inner wall of the tank body (1) through a second fixing frame (19), the outer side walls of the first liquid distribution ring (16), the second liquid distribution ring (17) and the third liquid distribution ring (18) are all communicated with a liquid supply pipe (20), and the liquid supply pipe (20) penetrates out of the side wall of the tank body (1), the end parts of the three liquid supply pipes (20) are communicated with a distribution pipe (21), the middle part of the distribution pipe (21) is communicated with a liquid inlet pipe (22), the tops of the first liquid distribution ring (16), the second liquid distribution ring (17) and the third liquid distribution ring (18) are respectively communicated with a vertical pipe (23) along the circumferential direction of the first liquid distribution ring, the second liquid distribution ring and the third liquid distribution ring, and the side wall of the vertical pipe (23) is uniformly provided with a plurality of through holes (24) along the circumferential direction and the axial direction of the vertical; the first liquid dividing ring (16), the second liquid dividing ring (17) and the third liquid dividing ring (18) are coaxially arranged and are positioned above the lower tube plate (5) and close to the lower tube plate (5).
6. The process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor according to claim 2, wherein two material distribution discs (25) are fixedly connected to the side surface of the inner wall of the upper end enclosure (3), the material distribution discs (25) are conical, and the top of each material distribution disc (25) is uniformly provided with a material inlet hole.
7. The process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor according to claim 2, wherein the bottom of the lower head (2) is communicated with a discharge port (8), the top of the upper head (3) is communicated with a feed port (9), the lower part of the side surface of the tank body (1) is communicated with three liquid inlet pipes (6), the three liquid inlet pipes (6) are uniformly distributed along the circumferential direction of the tank body (1), and the top of the side surface of the tank body (1) is communicated with a liquid outlet pipe (7).
8. The process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor according to claim 2, wherein the side wall of the upper tube plate (4) is fixedly connected with the top of the inner wall of the tank body (1), the side wall of the lower tube plate (5) is fixedly connected with the bottom of the inner wall of the tank body (1), and two ends of the tube array (12) respectively penetrate through the upper tube plate (4) and the lower tube plate (5) and are respectively fixedly connected with the upper tube plate (4) and the lower tube plate (5).
9. The process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor according to claim 2, wherein the top of the upper tube plate (4) and the bottom of the lower tube plate (5) are both provided with a coil (15), the bottom of the coil (15) at the top of the upper tube plate (4) is tightly attached to the top of the upper tube plate (4), one end of the coil (15) at the top of the upper tube plate (4) penetrates through the middle of the upper tube plate (4), the other end of the coil penetrates out of the tank body (1), the top of the coil (15) at the bottom of the lower tube plate (5) is tightly attached to the bottom of the lower tube plate (5), one end of the coil (15) at the bottom of the lower tube plate (5) penetrates through the middle of the lower tube plate (5), and the other end of the coil penetrates.
10. The process for preparing ethyl lactate by catalytic esterification of the fixed bed reactor according to claim 2, wherein a plurality of baffle plates (11) are arranged on the inner side wall of the tank body (1) and the side surfaces of the tubes (12); and the vertical pipes (23) of the auxiliary heat exchange assembly (13) are arranged between the tubes (12) and the tubes (12) in a penetrating manner.
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| CN204710282U (en) * | 2014-10-24 | 2015-10-21 | 中国石油化工股份有限公司 | For the fixed bed reactors of catalytic ammoniation legal system monoethanolamine |
| CN107033000A (en) * | 2016-02-03 | 2017-08-11 | 天津中福工程技术有限公司 | A kind of continuous liquid of fixed bed method that catalysis prepares lactate admittedly |
| CN107115827A (en) * | 2016-02-25 | 2017-09-01 | 亚申科技研发中心（上海）有限公司 | A kind of calandria type fixed bed reactor |
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| GB742931A (en) * | 1952-11-19 | 1956-01-04 | British Petroleum Co | Improvements in or relating to reactors |
| CN1736574A (en) * | 2005-07-08 | 2006-02-22 | 清华大学 | Non-hot spot calandria type fixed bed reactors |
| CN201151701Y (en) * | 2007-09-28 | 2008-11-19 | 任庚寅 | Novel chloroethylene synthesizing converter |
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