CN109593187A - A kind of large capacity solid phase polycondensation process - Google Patents
A kind of large capacity solid phase polycondensation process Download PDFInfo
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- CN109593187A CN109593187A CN201811531846.2A CN201811531846A CN109593187A CN 109593187 A CN109593187 A CN 109593187A CN 201811531846 A CN201811531846 A CN 201811531846A CN 109593187 A CN109593187 A CN 109593187A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/785—Preparation processes characterised by the apparatus used
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/80—Solid-state polycondensation
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application provides a kind of large capacity solid phase polycondensation process, belongs to preparation or the chemical process technology field of terephthalic acids esters high-molecular compound.Feed stock chip is sent into crystallizer, in 180-185 DEG C of circulation N2Under stirring, 5-30min is stopped in a crystallizer, and crystallizer outlet temperature is 175-182 DEG C；Slice after crystallization is sent into reactor, and reactor includes ridge conversion zone and at least two filling conversion zones, and end of reaction, output is the high-viscosity slicing of finished product.
Description
Technical field
This application involves a kind of large capacity solid phase polycondensation process, belong to terephthalic acids esters high-molecular compound preparation or
Chemical process technology field.
Background technique
Polyester slice with high viscosity is the raw material for producing polyester industrial fiber, and polyester low viscosity slice can be obtained by solid phase polycondensation
The polyester slice with high viscosity high to inherent viscosity, molecular weight is big.The production of polyester continuous solid phase thickening mostly uses fill-type, room at present
Ridge formula and fill-type and the concatenated two-part of ridge type.
Simple fill-type reaction system (using U.S. Bepex, toray as representative) needs mechanical stirring to crystallize, then through dry
After dry, preheater is heated to reaction temperature, into being viscosified in fill-type reactor.This processing route is long, and equipment is many and diverse, cuts
Piece easily agglomerates, and needs just prevent agglomeration material blocking pipeline using special discharging device.
Ridge type air hose is arranged in simple ridge type reaction system (being strangled with Switzerland's cloth as representative) in reactor, and material is made to exist
It is constantly overturn in reaction process, which alleviates the caking phenomenon of material in the reactor, but the device is complicated, and it is bulky,
Charging efficiency is low, and auxiliary device is more, and equipment manufacturing cost is higher.
Filled type and the concatenated two-part reaction system of ridge type combine the advantage of the two, are suitble to high yield weight polyester thickening
Production, but need that hot nitrogen conveying device is arranged between two sections, it is ensured that material transition is good, and engineering link is more, and land occupation is big, if
Standby maintenance is relatively more, is also easy to produce dust.
Summary of the invention
In view of this, the application provides a kind of achievable solid phase polycondensation process for being sliced large capacity, uniformly viscosifying.
Specifically, the application is realized by following scheme:
A kind of large capacity solid phase polycondensation process, the low viscous granulate metering as raw material is sent into crystallizer, at 180-185 DEG C
Circulation N2Under stirring, slice is advanced with jumping mode, and stops 5-30min in a crystallizer, and crystallizer outlet temperature is
175-182℃；Slice after crystallization is sent into reactor, and reactor includes ridge conversion zone and at least two filling conversion zones: institute
Ridge conversion zone is stated to recycle N2Heating maintains roof section reaction temperature at 200-220 DEG C；It is directly connected to ridge conversion zone
Filling conversion zone is kept the temperature with heating agent, N2Heating, N2Autoreactor lower end enters, and reactor temperature is 205-220 DEG C, and from upper
It is sequentially increased under and；The filling conversion zone being directly connected to reactor outlet is kept the temperature with heating agent, N2It is cooling, N2Autoreactor lower end
Into reactor temperature is 220-120 DEG C, and is successively reduced from top to bottom, end of reaction, and output, which is that the height of finished product is viscous, cuts
Piece (viscosity 0.90-1.25dl/g).
Solid-phase tack producing is divided into two major parts by the program: crystallization and reaction, in crystallized region, low viscous slice (viscosity 0.65 ±
0.05dl/g) in hot N2It realizes that the great-jump-forward of slice advances in reuse stirring, and completes the crystallization of feed stock chip in advance, really
The state that the slice reacted is in greater homogeneity is protected, uniformly viscosifies and lays the foundation for subsequent efficient, a large amount；Conversion zone then divides
For ridge conversion zone and filling conversion zone, the temperature of ridge conversion zone is controlled, and with cycling hot N2Slice is not only realized in heating
Pre- thickening, intrinsic viscosity increase between 0.80-0.92dl/g, also ensure the uniform progress of thickening, in filling conversion zone,
Filling conversion zone is again split into multistage, and with the hot N of adverse current uplink2Heating, the section continue to keep high temperature, it is ensured that warm from top to bottom
Degree is incremented by, and carries out slice segment and continues to increase, then continues to carry out slice thickening stage by stage, be large capacity slice thickening plus
Work provides possibility, when latter end is filled and reacted, in temperature range, guarantees that the temperature in this section of reactor is passed from top to bottom
Subtract, to end of reaction, temperature is reduced to 120-160 DEG C and nearby can directly discharge.Entire reaction can be achieved 240 ton/days
Yield (the Bu Leshi reactor daily output is only 40-60 ton/days, at present on the market maximum solid phase polycondensation up to 120t/D), no
Integration, procedure and the high yield of thickening reaction are only realized, and is sliced thickening uniformly, agglomeration will not be generated, completes to increase
Viscous to carry out finished product discharging, the viscosity of finished product is required up between 0.9-1.25dl/g according to different cultivars industrial yarn spinning
Setting, whole process need 20-40h, and uniformity is the undulated control between different batches within 0.025dl/g.
During the reaction, crystallization be solid-phase tack producing reaction basis, be based on above scheme, we to the process done into
The work of one step, and determine that the selection process of crystallization further includes being arranged as follows: slice is measured with revolving valve, and the revolving valve turns
Speed is 25-30r/min.The revolving speed of revolving valve controls the charging rate of slice, the charging rate and cycling hot N2Cooperation, it is ensured that
Slice stable can be stopped in a crystallizer with state of jumping, and therefore, during entire crystallization, slice is existed in dynamic
, avoid because heat it is irregular caused by slice crystallize not uniform slice caking phenomenon.
During the reaction, the pre- thickening section as the thickening core stage, it is anti-with filling that ridge conversion zone has been connected crystallization
Section is answered, is based on above scheme, we have done further work to the process, and determine the selection process of ridge conversion zone also
Including being arranged as follows: slice is measured with revolving valve, and the revolving valve revolving speed is 25-30r/min.The revolving speed of revolving valve controls
The charging rate of slice, the charging rate and cycling hot N2Cooperation, it is ensured that slice can guarantee in thickening stage thermally equivalent in advance
During entire pre- thickening, slice is all heated in dynamic, avoid because be sliced viscosify in advance it is irregular caused by slice caking phenomenon.More
Preferably, N is recycled2Temperature is 205-220 DEG C, pressure 10-15kPa, and dew point -90~-50 DEG C, oxygen content is less than 10ppm, flow
120-130Nm3/min。
During the reaction, the main thickening section as the thickening core stage, filling conversion zone are divided into multistage progress, are based on
Above scheme, we have done further work to the process, and determine that the selection process of filling conversion zone further includes as follows
Setting: filling conversion zone, which includes at least, two sections, and first section filling reaction and latter end filling reaction are all made of revolving valve discharging, revolution
Valve revolving speed 15-20r/min.It is furthermore preferred that heating agent uses conduction oil, temperature is 200-230 DEG C.Heating agent complex reaction device carries out temperature
The control of degree, in mildly circulation N2Under the conditions of, it is ensured that reaction environment temperature.
On the basis of the studies above, based on the characteristic of individual materials, we are additionally provided with cooling section at reactor rear,
To ensure drop temperature.
On the basis of the studies above, we are also studied entire solid-phase polymerization system, and the preferably solid phase
The reaction unit that polycondensating process uses includes crystallizer, ridge conversion zone and multiple filling conversion zones, the crystallizer entrance
Setting crystallization revolving valve carries out feed stock chip charging, and exit setting crystallization discharging revolving valve expects crystallization to be sent into ridge reaction
Section, crystallizer are fitted with crystallization nitrogen tube, and the setting crystallization nitrogen separation device in crystallization nitrogen tube, realize N2Circulation
Reflux supply；Ridge conversion zone and multiple filling conversion zones are integral type connectivity structure, and ridge conversion zone is divided into more piece, adjacent segments
Between heated with heater, ridge conversion zone is fitted with reaction nitrogen tube, and reaction nitrogen tube is from ridge conversion zone bottom
Portion is fed, top output, is reacted setting reaction nitrogen separation device in nitrogen tube, is realized N2Circulating reflux supply；Multiple fillings
It include the latter end filling that first section filling reactor, the setting reactor being directly connected to ridge conversion zone integrally export in conversion zone
Multiple interludes between reactor and setting and first section filling reactor and latter end filling reactor fill reactor, and filling is anti-
Answer each section of outer wall of device with the heat preservation of heating agent coil pipe, each section is respectively set nitrogen inlet and carries out hot N2It feeds, each nitrogen inlet is located at
The lower end of corresponding segment.
Above-mentioned apparatus is fed to height from low viscous feed stock chip and sticks into product slice output, is to complete in the reactor, reaction
In device, ridge conversion zone and multiple filling conversion zones are integral type connectivity structure, realize being carried out continuously for material thickening process,
Effectively increase the stability of reaction efficiency and reaction environment, different sections (including ridge conversion zone and first section filling reactor with
And between adjacent segment filling inside reactor) between mutually indepedent temperature control and pressure control, realize that the segmentation of slice viscosifies step by step.
Further, as preferred:
The just section filling reactor includes Ta Gai, tower section, middle tube, shell ring and cone, Ta Gai, tower section, middle tube, cylinder
Section, cone are sequentially connected with, and slice entrance is set to tower tops, and heating agent coil pipe disk is set to shell ring outer wall, and nitrogen inlet is set to
Cone side wall, the outlet of cone base setting slice.It is furthermore preferred that insulating layer, heat preservation is arranged in the just section filling reactor outer wall
Layer is made of alumina silicate fibre, glass cloth and galvanized steel plain sheet.Setting distribution cone between the cone and shell ring, it is ensured that slice is smooth
Output.The middle tube is using hemispherical dome pipe, in transfer of forming a connecting link, it is ensured that slice circulation is smooth.The shell ring is provided with
Temperature tube, temperature tube are respectively set at shell ring different height, and for monitoring the temperature in shell ring in real time, thermometric pipe outer wall is preferred
Casing is set, and casing had not only facilitated the installation of temperature tube, but also shell ring outside wall temperature is avoided to do to caused by the measurement of temperature tube temperature
It disturbs；Temperature tube relative level is obliquely installed.The cone angle θ is 30-80 °.
The latter end fills multiple shell rings that reactor includes end socket and is set to below end socket, and heating agent coil pipe disk is set to cylinder
Outer wall is saved, cone is arranged in shell ring end, and nitrogen inlet is set to shell ring lower part, and cone base picks out discharge nozzle.It is furthermore preferred that institute
It states between adjacent cylindrical section with link of boards, inner cylinder is set on gusset, the channel as heating agent coil pipe；The latter end shell ring is provided with
Component is bored in upper dispersion cone component and lower dispersion, and upper dispersion cone component is bored between end shell ring and shell ring adjacent thereto
Sharp upward, lower dispersion cone component is between end shell ring and cone, and cone is downward；Upper dispersion cone component and lower dispersion cone group
The setting of part forms the discharging of multiple tracks ladder, facilitates the smooth progress that in high volume discharges.The shell ring is provided with temperature tube, temperature tube
It is respectively set at shell ring different height, for monitoring the temperature in shell ring in real time, thermometric pipe outer wall is preferably provided with casing, casing
Not only the installation of temperature tube had been facilitated, but also has avoided shell ring outside wall temperature to interference caused by the measurement of temperature tube temperature；Temperature tube is opposite
Horizontal plane is obliquely installed.The cone angle beta of the cone is 30-80 °.
Detailed description of the invention
Fig. 1 is the overall flow schematic diagram of the application；
Fig. 2 is the positive structure schematic of one section of filling reactor in the application；
Fig. 3 is the side structure schematic diagram of one section of filling reactor in the application；
Fig. 4 is the direction A-A view in Fig. 2；
Fig. 5 is the overlooking state schematic diagram of one section of filling reactor in the application；
Fig. 6 is the side structure schematic diagram of two sections of filling reactors in the application；
Fig. 7 is the partial enlarged view at the position B in Fig. 6；
Fig. 8 is C direction view (not to scale (NTS) enlarged drawing) in Fig. 7；
Fig. 9 is the welding detail drawing in Fig. 6 at temperature tube；
Figure 10 is the connection orientation in two sections of filling reactors.
Figure label: 1. crystallizers；11. feeding revolving valve；12. material inlet；13. crystallizing nitrogen tube；14. crystallizing nitrogen
Gas separating device；15. crystallization discharging revolving valve；2. ridge conversion zone；21. first segment；22. the second section；23. third section；24. the 4th
Section；25. heater；26. reacting nitrogen tube；27. reacting nitrogen separation device；3. one section of filling reactor；31. one section of heating agent disk
Pipe；311. 1 sections of Heating mediums；312. 1 sections of heating agent outlets；32. tower lid；321. 1 sections of slice imports；33. tower section；331. nitrogen
Gas entrance；332. nitrogen outlet；Tube in 34.；341. gussets one；35. one section of shell ring；36. one section of cone；361. 1 sections of nitrogen
Pipe；37. one section of temperature tube；38. distribution cone；4. two sections of filling reactors；41. two sections of heating agent coil pipes；42. end socket；421. 2 sections
Feed pipe；43. two sections of shell rings；431. shell rings one；432. shell rings two；433. shell rings three；434. shell rings four；Disperse cone group on 435.
Part；436. lower dispersion cone components；437. cones one；438. lacing wire；439. block；44. inner cylinder；441. gussets two；45. cone
Guide collar；46. two sections of supplement imports；47. cone two；48. two sections of discharge nozzles；49. two sections of temperature tubes；491. casing；5. finished product
Discharge nozzle；51. discharge revolving valve.
Specific embodiment
A kind of large capacity solid phase polycondensation process of the present embodiment, the low viscous granulate metering as raw material are sent into crystallizer,
180-185 DEG C of circulation N2Under stirring, slice is advanced with jumping mode, and stops 5-30min in a crystallizer, crystallizer outlet
Temperature is 175-182 DEG C；Slice after crystallization is sent into reactor, and reactor includes ridge conversion zone and at least two filling reactions
Section: the ridge conversion zone is to recycle N2Heating maintains roof section reaction temperature at 200-210 DEG C；It is direct with ridge conversion zone
The filling conversion zone of connection is kept the temperature with heating agent, N2Heating, N2Autoreactor lower end enters, and reactor temperature is 205-210 DEG C,
And it is sequentially increased from top to bottom；The filling conversion zone being directly connected to reactor outlet is kept the temperature with heating agent, N2It is cooling, N2Autoreaction
Device lower end enters, and reactor temperature is 210-160 DEG C, and is successively reduced from top to bottom, end of reaction, and output is finished product
High-viscosity slicing.
Solid-phase tack producing is divided into two major parts by the program: crystallization and reaction, and in crystallized region, low viscous slice is in hot N2Reuse stirring
The middle great-jump-forward for realizing slice advances, and the crystallization of feed stock chip is completed in advance, it is ensured that the slice reacted is in product
The uniform state of matter is uniformly viscosified and is laid the foundation for subsequent efficient, a large amount；Conversion zone is then divided into ridge conversion zone and filling reaction
Section controls the temperature of ridge conversion zone, and with cycling hot N2Heating, not only realizes the pre- thickening of slice, also ensures thickening
It uniformly carries out, in filling conversion zone, filling conversion zone is again split into multistage, and with the hot N of adverse current uplink2Heating, the Duan Ji
High temperature is held in continuation of insurance, it is ensured that temperature increment from top to bottom carries out slice segment and continues to increase, then continues to be sliced stage by stage
Thickening provides possibility for the slice thickening processing of large capacity, when latter end is filled and reacted, in temperature range, guarantees the section
Temperature in reactor is successively decreased from top to bottom, and to end of reaction, temperature is reduced to 160 DEG C and nearby can directly discharge.Entirely
Integration, procedure and the high yield that reaction not only realizes thickening reaction carry out, but also are sliced thickening uniformly, will not generate knot
Block, finished product discharging can be carried out by completing thickening.
Wherein, during the reaction, crystallization is the basis of solid-phase tack producing reaction, therefore above scheme can also be according to as follows
Mode is added: slice is measured with revolving valve, and the revolving valve revolving speed is 25-27r/min.The revolving speed of revolving valve controls slice
Charging rate, the charging rate and cycling hot N2Cooperation, it is ensured that slice stable can be stopped in a crystallizer with state of jumping,
Therefore, during entire crystallization, slice be all in existing for dynamic, avoid because heat it is irregular caused by slice crystallization is not uniform cuts
Piece caking phenomenon.
During the reaction, the pre- thickening section as the thickening core stage, ridge conversion zone have been connected crystallization and have increased with filling
Viscous section, therefore above scheme can also add as follows: slice is measured with revolving valve, and the revolving valve revolving speed is 25-
27r/min.The revolving speed of revolving valve controls the charging rate of slice, the charging rate and cycling hot N2Cooperation, it is ensured that slice energy
Enough in thickening stage thermally equivalent in advance, during guaranteeing entire pre- thickening, slice is all heated in dynamic, avoids because being sliced pre- thickening
Slice caking phenomenon caused by irregular.It is furthermore preferred that circulation N2Temperature is 205-215 DEG C, pressure 10-15kPa, dew point -70
DEG C, oxygen content 2-6ppm, flow 120-130Nm3/min。
During the reaction, the main thickening section as the thickening core stage, filling thickening section are divided into multistage progress, therefore
Above scheme can also add as follows: filling conversion zone, which includes at least, two sections, and first section filling reaction and latter end are filled out
It fills reaction and is all made of revolving valve discharging, revolving valve revolving speed 15-20r/min.It is furthermore preferred that heating agent uses conduction oil, temperature is
200-230℃.Heating agent complex reaction device carries out the control of temperature, in mildly circulation N2Under the conditions of, it is ensured that reaction environment temperature.
As the concrete case of above scheme, it (includes four sections, filling with ridge conversion zone that the above process, which can be described as follows,
Conversion zone is including for two sections):
Crystallization: low adhesive aggregation ester slice measures (revolving speed 26r/min) at room temperature, through revolving valve, into crystallizer, in crystallizer
With 183.2 DEG C of hot N2Agitation slice, makes slice advance in a jumped fashion, and residence time 5-30min is sliced outlet temperature
It is 180.1 DEG C；Hot nitrogen reuse after cyclonic separation.
Ridge conversion zone: temperature is 172.7 DEG C when slice enters, and revolving valve revolving speed is 26r/min.From first segment to the 4th
Reactor is saved, maintains temperature at 210 DEG C or so, is heated by hot nitrogen.Nitrogen process parameter are as follows: 212 DEG C, 11.1kPa,
122.5Nm3/min；Hot nitrogen is recycled after cyclonic separation regenerates in systems.
Fill conversion zone 1 (i.e. just section): barrel type reactor, surrounding are kept the temperature with heating agent coil pipe, and 210 DEG C of inlet temperature.Heat
Nitrogen enters reactor from lower end, and 215 DEG C.Slice is come out by revolving valve, 16r/min.Reactor temperature is at 210-215 DEG C
Left and right, is sequentially increased from top to bottom.
Fill conversion zone 2 (i.e. latter end): barrel type reactor, surrounding are kept the temperature with heating agent coil pipe, and 214 DEG C of inlet temperature；It is cold
But nitrogen enters reactor from lower end, and 80 DEG C of inlet temperature, 214 DEG C of outlet temperature.Slice is gone out by revolving valve, 16r/min.Instead
Temperature in device is answered successively to reduce from top to bottom, from 172.3 DEG C to 70.9 DEG C, discharging.
On the basis of the studies above, based on the characteristic of individual materials, we are additionally provided with cold in reactor rear/lower section
But section, to ensure drop temperature.
On the basis of the studies above, we are also studied entire solid-phase polymerization system, in conjunction with Fig. 1, in determination
The reaction unit for stating solid phase polycondensation process use includes crystallizer 1, ridge conversion zone 2 and multiple filling conversion zones, crystallization substantially
Setting crystallization revolving valve 11 carries out feed stock chip charging, exit setting crystallization discharging revolving valve 15 at the material inlet 12 of device 1
Crystallization is expected to be sent into ridge conversion zone 2, crystallizer 1 is fitted with crystallization nitrogen tube 13, and is arranged in crystallization nitrogen tube 13
Nitrogen separation device 14 is crystallized, realizes N2Circulating reflux supply；Ridge conversion zone 2 is that integral type is connected to multiple filling conversion zones
Structure, ridge conversion zone 2 include first segment 21, the second section 22, third section 23, Section 4 24, first segment 21 and the second section 22,
Second section 22 is heated respectively with heater 23 with third section 23, third section 23 with Section 4 24, the cooperation peace of ridge conversion zone 2
Equipped with reaction nitrogen tube 26, reaction nitrogen tube 26 exports, reaction from Section of 4 24 entrance of ridge conversion zone 2 from first segment 21
Setting reaction nitrogen separation device 27, realizes N in nitrogen tube 262Circulating reflux supply；Include in multiple filling conversion zones and room
Latter end filling reactor that first section that ridge conversion zone 2 is directly connected to filling reactor, setting reactor integrally export and setting with
Multiple interludes between first section filling reactor and latter end filling reactor fill reactor, and filling each section of outer wall of reactor is equal
With the heat preservation of heating agent coil pipe, each section is respectively set nitrogen inlet and carries out hot N2It feeds, each nitrogen inlet is located at corresponding segment lower end.
Above-mentioned apparatus is fed to height from low viscous feed stock chip and sticks into product slice output, is substantially and completes in the reactor,
In reactor, ridge conversion zone 2 and multiple filling conversion zones are integral type connectivity structure, realize the continuous of material thickening process
Carry out, effectively increase the stability of reaction efficiency and reaction environment, different sections (including ridge conversion zone and the filling of first section it is anti-
Answer device and adjacent segment to fill between inside reactor) between mutually indepedent temperature control and pressure control, realize that the segmentation of slice increases step by step
It is viscous.
Preferably, above-mentioned apparatus can also add as follows: filling reactor includes two sections, i.e., one section filling
Reactor 3 (i.e. just section fills reactor, similarly hereinafter) and two sections of filling reactors 4 (i.e. latter end fills reactor, similarly hereinafter), one section is filled out
It fills reactor 3 to be connected to ridge conversion zone 2, two sections of 4 upper ends of filling reactor are connected to one section of filling reactor 3, and lower end picks out
Finished product discharge nozzle 5, and finished product revolving valve 51 is set on finished product discharge nozzle 5 and is discharged.
Further, in conjunction with Fig. 2 and Fig. 3, one section of filling reactor 3 includes tower lid 32, tower section 33,34, one sections of middle tube
Shell ring 35 and one section of cone 36, tower lid 32, tower section 33,34, one sections of shell rings 35 of middle tube and one section of cone 36 are sequentially connected with, and one
Section slice entrance 321 is set to 32 top of tower lid, and is connected to crystallizer 2；One section of 31 disk of heating agent coil pipe is set to one section of shell ring 35
Outer wall, one section of nitrogen tube 361 are set to one section of 36 side wall of cone, the setting slice outlet of one section of 36 bottom of cone.
Above-mentioned one section of filling reactor 3 is further provided that the outer wall setting insulating layer (figure of one section of filling reactor 3
In do not mark), insulation layer thickness 200mm is made of alumina silicate fibre, glass cloth and 0.5mm galvanized steel plain sheet.
Above-mentioned one section of filling reactor 3 is further provided that in conjunction with Fig. 3, between one section of cone 36 and one section of shell ring 35
Setting distribution cone 38, it is ensured that be sliced smooth output.
Above-mentioned one section of filling reactor 3 is further provided that middle tube 34 uses hemispherical dome pipe, transfer of forming a connecting link
In, it is ensured that slice circulation is smooth.Middle 34 outer wall of tube is preferably provided with gusset 1, it is ensured that installation is stablized.
Above-mentioned one section of filling reactor 3 is further provided that one section of shell ring 35 is provided with one section of temperature tube 37, one section of survey
Warm pipe 37 is respectively set at one section of 35 different height of shell ring, for monitoring the temperature in one section of shell ring 35, one section of thermometric in real time
37 outer wall of pipe is preferably provided with casing (being not marked in figure, can refer to Fig. 9), and casing had not only facilitated the installation of temperature tube, but also avoided one
Section 35 outside wall temperature of shell ring interferes caused by measuring one section of 37 temperature of temperature tube；One section of 37 relative level of temperature tube inclination is set
It sets.
Above-mentioned one section of filling reactor 3 is further provided that in conjunction with Fig. 3, one section of 36 θ of cone is 50 °.
In the installation that above-mentioned one section is filled reactor 3, it is related to the installation of multiple pipe fittings and accessory, setting angle carries out
It is preferably provided with as follows: in conjunction with Fig. 4, a temperature tube is filled at 180 °, four temperature tubes are filled at 225 °, two samplings are filled at 270 °
Mouthful, one section of nitrogen tube 361 is filled at 315 °；Nitrogen tube, the nitrogen inlet 331 and nitrogen outlet of nitrogen tube are set in 33 outer wall disk of tower section
332 be in shift to install as shown in Figure 5.
Further, in conjunction with Fig. 6, two sections of filling reactors 4 include that end socket 42 (for convenience of installation and material transferring, uses
Ellipse head) and multiple two sections of shell rings 43 of the lower section of end socket 42 are set to, end socket 42 is filled by two section feeding pipes 421 with one section
The slice outlet of reactor 3；Two sections of 41 disks of heating agent coil pipe are set to two sections of 43 outer walls of shell ring, and cone is arranged in two sections of shell ring ends
One 437, one 437 bottom of cone picks out two sections of discharge nozzles 48, and two sections of discharge nozzles 48 are connected to finished product discharge nozzle 5.Specific to this case
In example, two sections of shell rings 43 include shell ring 1, shell ring 2 432, shell ring 3 433, shell ring 4 434, shell ring 1, shell ring two
432, shell ring 3 433, shell ring 4 434 are interconnected, one 431 upper ends of shell ring, that is, end socket 42,4 434 lower end of shell ring and cone one
437 connections.
Above-mentioned two sections of fillings reactor 4 is further provided that between adjacent cylindrical section with the connection of gusset 2 441, gusset two
Inner cylinder 44 is set on 41, and inner cylinder 44 is the channel of two sections of heating agent coil pipes 41.
Above-mentioned two sections of fillings reactor 4 is further provided that two sections of shell rings 43 are provided with two sections of temperature tubes 49, two sections of surveys
Warm pipe 49 is respectively set at shell ring different height, for monitoring the temperature in shell ring in real time, in conjunction with Fig. 9, two sections of temperature tubes 49
Outer wall is preferably provided with casing 491, and casing 491 had not only facilitated the installation of two sections of temperature tubes 49, but also avoided shell ring outside wall temperature to two
It is interfered caused by section 49 temperature of temperature tube measurement；Two sections of 49 relative level of temperature tube are obliquely installed.
Above-mentioned two sections of fillings reactor 4 is further arranged to: in conjunction with Fig. 6, one 437 angle beta of cone is 50 °.
Above-mentioned two sections of fillings reactor 4 is further provided that, in conjunction with Fig. 7, the lower part of shell ring 1 is provided with lacing wire
438, block 439 is set at arrow C；And the corresponding 438 lower section heaving pile pipe orientation of lacing wire arrow C (is not marked with hand hole in figure
Note), that nozzle direction (is not marked in figure) in feed liquid hole is consistent.
Above-mentioned two sections of fillings reactor 4 is further provided that in conjunction with Fig. 6, between shell ring 1 and shell ring 2 442
Cone guide collar 45 is set.
Above-mentioned two sections of fillings reactor 4 is further provided that in conjunction with Fig. 6, and two sections of supplement imports are arranged at shell ring 3 433
46, carry out the supplement of nitrogen.
Above-mentioned two sections of fillings reactor 4 is further provided that, in conjunction with Fig. 6,3 433 bottom of shell ring is downwardly extending cone
Body 2 47.
Above-mentioned two sections of fillings reactor 4 is further provided that in conjunction with Fig. 6, dispersion cone component in the setting of shell ring 4 434
435 and lower dispersion bore component 436；For upper dispersion cone component 435 between shell ring 4 434 and shell ring 3 433, cone is upward；Under
For dispersion cone component 436 between shell ring 4 434 and cone 1, cone is downward.
In the installation of two sections of filling reactors 4, it is related to the installation of multiple pipe fittings and accessory, setting angle is provided that
In conjunction with Figure 10,0 °, 180 °: two section Heating mediums, two sections of heating agent outlets；45 °: two sections of supplement imports 46, exhaust outlets (are not marked in figure
Note)；135 °: visor；170 °: hand hole；225 °: four temperature tubes；247.5 °: four temperature tubes；270 °: four temperature tubes；
292.5 °: sample tap, feed liquid meter mouth；315 °: air inlet.
Claims (10)
1. a kind of large capacity solid phase polycondensation process, it is characterised in that: the low viscous granulate metering as raw material is sent into crystallizer,
180-185 DEG C of circulation N2Under stirring, slice is advanced with jumping mode, and stops 5-30min in a crystallizer, crystallizer outlet
Temperature is 175-182 DEG C；Slice after crystallization is sent into reactor, and reactor includes ridge conversion zone and at least two filling reactions
Section: the ridge conversion zone is to recycle N2Heating maintains roof section reaction temperature at 200-220 DEG C；It is direct with ridge conversion zone
The filling conversion zone of connection is kept the temperature with heating agent, N2Heating, N2Autoreactor lower end enters, and reactor temperature is 205-220 DEG C,
And it is sequentially increased from top to bottom；The filling conversion zone being directly connected to reactor outlet is kept the temperature with heating agent, N2It is cooling, N2Autoreaction
Device lower end enters, and reactor temperature is 220-120 DEG C, and is successively reduced from top to bottom, end of reaction, and output is finished product
High-viscosity slicing.
2. a kind of large capacity solid phase polycondensation process as described in claim 1, it is characterised in that: in Crystallization Procedure, slice is to return
Rotary valve metering, the revolving valve revolving speed are 25-30r/min.
3. a kind of large capacity solid phase polycondensation process as described in claim 1, it is characterised in that: in ridge conversion zone, slice with
Revolving valve metering, the revolving valve revolving speed are 25-30r/min.
4. a kind of large capacity solid phase polycondensation process as described in claim 1, it is characterised in that: in ridge conversion zone, recycle N2Temperature
Degree is 205-220 DEG C, pressure 10-15kPa, flow 120-130Nm3/ min, dew point -90~-50 DEG C.
5. a kind of large capacity solid phase polycondensation process as described in claim 1, it is characterised in that: filling conversion zone, which includes at least, to be had
Two sections, first section filling reaction and latter end filling reaction are all made of revolving valve discharging, revolving valve revolving speed 15-20r/min.
6. a kind of large capacity solid phase polycondensation process as described in claim 1, it is characterised in that: in filling conversion zone, heating agent is adopted
With conduction oil, temperature is 200-230 DEG C.
7. a kind of large capacity solid phase polycondensation process as claimed in any one of claims 1 to 6, it is characterised in that: solid phase polycondensation process
The reaction unit of use includes crystallizer, ridge conversion zone and multiple filling conversion zones, the crystallizer entrance setting crystallization
Revolving valve carries out feed stock chip charging, and exit setting crystallization discharging revolving valve expects crystallization to be sent into ridge conversion zone, crystallizer
It is fitted with crystallization nitrogen tube, and the setting crystallization nitrogen separation device in crystallization nitrogen tube, realizes N2Circulating reflux supply；
Ridge conversion zone and multiple filling conversion zones are integral type connectivity structure, and ridge conversion zone is divided into more piece, to add between adjacent segments
Hot device is heated, and ridge conversion zone is fitted with reaction nitrogen tube, and reaction nitrogen tube is fed from ridge conversion zone bottom, top
Portion's output reacts setting reaction nitrogen separation device in nitrogen tube, realizes N2Circulating reflux supply；It is wrapped in multiple filling conversion zones
Include the latter end filling reactor and set that first section filling reactor, the setting reactor being directly connected to ridge conversion zone integrally export
The multiple interludes filling reactor being placed between first section filling reactor and latter end filling reactor, each section of filling reactor are outer
With the heat preservation of heating agent coil pipe, each section is respectively set nitrogen inlet and carries out hot N wall2It feeds, each nitrogen inlet is located under corresponding segment
End.
8. a kind of large capacity solid phase polycondensation process as claimed in claim 7, it is characterised in that: the just section fills reactor packet
Ta Gai, tower section, middle tube, shell ring and cone are included, Ta Gai, tower section, middle tube, shell ring, cone are sequentially connected with, slice entrance setting
In tower tops, heating agent coil pipe disk is set to shell ring outer wall, and nitrogen inlet is set to cone side wall, and cone base setting is sliced out
Mouthful.
9. a kind of large capacity solid phase polycondensation process as claimed in claim 7, it is characterised in that: the latter end fills reactor packet
The multiple shell rings for including end socket and being set to below end socket, heating agent coil pipe disk are set to shell ring outer wall, and cone, nitrogen is arranged in shell ring end
Entrance is set to shell ring lower part, and cone base picks out discharge nozzle.
10. a kind of large capacity solid phase polycondensation process as claimed in claim 9, it is characterised in that: the latter end shell ring is provided with
Component is bored in upper dispersion cone component and lower dispersion, and upper dispersion cone component is bored between end shell ring and shell ring adjacent thereto
Sharp upward, lower dispersion cone component is between end shell ring and cone, and cone is downward.
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| CN102295764A (en) * | 2011-07-11 | 2011-12-28 | 大连海新工程技术有限公司 | Process of integrated ridge-filling reactor for polyester solid-phase tackification |
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