CN104277211B - Four still polyplants - Google Patents
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- CN104277211B CN104277211B CN201410505447.4A CN201410505447A CN104277211B CN 104277211 B CN104277211 B CN 104277211B CN 201410505447 A CN201410505447 A CN 201410505447A CN 104277211 B CN104277211 B CN 104277211B
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Abstract
The present invention relates to a kind of four still polyplants, belong to high molecular polymerization device technique field.Including esterifying kettle one, esterifying kettle two, precondensation still and whole polycondensation vessel, esterifying kettle one is made up of kettle, the sleeve being arranged in kettle and coil pipe one, and sleeve wall arranges multiple through hole, and kettle is connected by through hole with sleeve；Esterifying kettle two is made up of mistress, interior room and the coil pipe two that is arranged in interior room；Precondensation still is upper room and the vertical structure of lower room composition；Whole polycondensation vessel is made up of squirrel-cage agitator one and squirrel-cage agitator two.This device being applied to PET polymerization process, not only achieves the significantly lifting of intrinsic viscosity, be conducive to the optimization of the serviceabilities such as subsequent product machinery, and course of reaction is more terse, whole efficiency improves, it may be achieved single covering device vast capacity produces.
Description
Technical field
The present invention relates to a kind of four still polyplants, belong to high molecular polymerization device technique field.
Background technology
PET section or melt are the high molecular polymers formed through over-churning dehydration aftercondensated by raw material p-phthalic acid and ethylene glycol, it includes successively in the course of processing, and esterification one, esterification two, precondensation one, precondensation two and final minification are poly-to be constituted, and precondensation therein carries out in two reactors.The advantage of this mode is in that reaction operation comparatively steady, convenient, but shortcoming is in that in its two steps precondensation to be required higher to intrinsic viscosity control, could enter in precondensation two as precondensation one intrinsic viscosity reaches about 0.15dl/g, then gather then through final minification, intrinsic viscosity is increased to about 0.68dl/g, then again through solid-phase tack producing, intrinsic viscosity is increased to about 1.0dl/g.Polyester process ripe at present has Ji Ma, Yi Wenda, clock to spin the three still polymerization process adopting five still polymerization process and Du Pont to adopt, wherein five autoclaves process adopts the temperate condition of low mole prop0rtion [n (EG): n (PTA)=1.10-1.20:1], low-temperature atmosphere-pressure, response time is long, product performance index is stable, diethylene glycol content is low, colour is low and stable, is the polyplant of main flow；Du Pont three still flow process adopts high molar ratio [n (EG): n (PTA)=1.80-2.00:1], high temperature, fine vacuum reaction condition, its shortcoming is in that, the excessive meeting of EG makes the content of diethylene glycol in course of reaction raise, and high temperature reaction for a long time can make melt b value raise, reaction process is too short makes product quality fluctuation big, the window narrows adjusted in production process.Whether the advantage of the two can be combined, a kind of low mole prop0rtion of exploitation, gentle and shorter technological process so that constant product quality, production process is easy to control is the target in PET industry.Based on this, make subject application.
Summary of the invention
In order to overcome technological process length existing for esterification mode, complex procedures, the present invention provides a kind of and is esterified intrinsic viscosity height, stable reaction, process-cycle short four still polyplants.
For achieving the above object, the technical scheme that the present invention takes is as follows:
Four still polyplants, including esterifying kettle one, esterifying kettle two, precondensation still and whole polycondensation vessel, described esterifying kettle one is made up of kettle, the sleeve being arranged in kettle and coil pipe one, coil pipe one extends from the bottom up of kettle and is surrounded between sleeve and kettle, sleeve wall arranges multiple through hole, kettle is connected by through hole with sleeve, arranges agitator one in sleeve；Described esterifying kettle two is made up of mistress, interior room and the coil pipe two that is arranged in interior room, obstructed bottom mistress and interior room, and interior room sidewall arranges hole, mistress is connected by hole with interior room, it is provided with support bar between mistress and interior room, to support interior room cylinder, interior room arranges agitator two；Described precondensation still is vertical structure, including upper room and lower room, upper room is obstructed with lower room, and described upper room is divided into multiple annular compartment by helical baffle, arranges coil pipe three in compartment, the compartment place in bosom, upper room is provided with communicating pipe, melt in upper room, through sending into lower room communicating pipe, arranges thermometer, is provided with agitator three in precondensation still in this communicating pipe, agitator three is arranged in lower room, arranges coil pipe four in lower room；Described whole polycondensation vessel is made up of squirrel-cage agitator one and squirrel-cage agitator two, it is provided with multiple Dropbox being parallel to each other at squirrel-cage agitator one and squirrel-cage agitator two, Dropbox is installed in whole polycondensation vessel framework by rotating shaft, and in squirrel-cage agitator one, Dropbox distribution density is big compared with Dropbox distribution density in squirrel-cage agitator two；The material inlet of esterifying kettle one is positioned at kettle top, the bottom of esterifying kettle one is communicated in the middle part of the mistress of esterifying kettle two by connecting tube one, the bottom of esterifying kettle two is communicated in the compartment that on precondensation still, in room, outermost layer helical baffle is formed by connecting tube two, precondensation bottom portion connected connecting tube tee joint squirrel-cage agitator one bottom to whole polycondensation vessel, and discharged material through the bottom of squirrel-cage agitator two.
Further, as preferably:
In described esterifying kettle one, coil pipe one, for going with each other all the time, is from bottom to top disposed with five groups, and first group is two-layer, and second group is three layers, and the 3rd group is four layers, and the 4th group is five layers, and the 5th group is six layers, totally two ten layers.Being more highly preferred to, often the spacing between group coil pipe one is 10cm-50cm.
In described esterifying kettle two, coil pipe two is provided with ten groups, and its concrete set-up mode is layered laminate arrangement.
In described precondensation still, in lower room, coil pipe is provided with six floor, and its concrete set-up mode is for going with each other all the time, with layered laminate arrangement；In upper room, liquidometer adopts bubble liquid level meter, and in lower room, liquidometer adopts radioactive source liquidometer.
In precondensation still, according to the size to the requirement of precondensation still intrinsic viscosity and kettle diameter, dividing plate may be configured as 2-8 circle, and dividing plate is provided with agnail plate, forms the mixed effect in circulation process increasing fluid.
Described Dropbox is made up of housing, net bar, mesh and internal ring, and internal ring is arranged with housing concentric, and net bar is crisscross arranged between housing and internal ring, and staggered net bar forms mesh, and Dropbox passes through internal ring and rotating shaft；In described whole polycondensation vessel, the cross-shaped state of net bar of adjacent two panels Dropbox, to improve Surface Renewal efficiency during stirring.Wherein, between net bar and net bar can be orthogonal being crisscross arranged, it is also possible to for being crisscross arranged at an angle, can be some fixing spacing between adjacent net bar, it is also possible to be gradual change or indefinite a certain spacing, to adapt to different stirring demand.
Raw material p-phthalic acid and ethylene glycol are proportionally added into catalyst and are configured to slurry, added by esterifying kettle one top, slurry enters after in still, agitator one is pressed downward against, slurry via through holes circulates back and forth between sleeve and kettle, after carrying out first stage esterification, carboxylate is by being drained in the mistress of esterifying kettle two bottom esterifying kettle one, and room in the hole entrance on interior room, complete the carboxylate after second stage esterification and be delivered in the upper room of precondensation, after material circulates in the compartment that helical baffle is formed, through sending into lower room communicating pipe, complete prepolymerization reaction；This prepolycondensate is sent into reaction in whole polycondensation vessel, the whole polycondensation product of final acquisition.
Compared with five conventional stills, six still polymerization methodses, beneficial effects of the present invention and operation principle are as follows:
1. the intensive degree of equipment improves.Reactor total quantity reduces, and installation footprint reduces, and equipment investment cost is low.In five common still polymerization methodses, need to be equipped with esterifying kettle one, esterifying kettle two, precondensation still one, precondensation still two, whole polycondensation vessel totally five kettlies, the installation in one line of these kettlies, not only floor space is big, and in installation process, it is necessary to it is equipped with substantial amounts of connecting tube, circuit and corresponding heating agent；And in the present invention, kettle used only needs esterifying kettle one, esterifying kettle two, precondensation still and whole four stills of polycondensation vessel, precondensation still therein adopts upper and lower mutual disconnected vertical structure, this structure makes equipment integral installation area reduce 1/5, and heating agent makes consumption also be controlled, integral production cost can reduce 30-50%.
2. the efficiency of package unit improves, and handling promotes, it may be achieved single covering device vast capacity produces.Adopting this device, Zhejiang Guxiandao Industrial Fiber Co., Ltd. achieves the Large Copacity device producing 500000 tons of polyester per year, whole process reaction time decreased, and device efficiency promotes, and simultaneous reactions still quantity reduces, and operation site is reduced.
3. in bulk polymerization process, intrinsic viscosity is obviously improved, and shortens the response time, is conducive to the raising of subsequent product processing characteristics.nullIn polymerization technique provided by the present invention，When carboxylate enters into precondensation stage，It is introduced in the compartment in room，In this compartment，Carboxylate is circulated conveying along specific track，The process of conveying completes the initial reaction of precondensation，And achieve the lifting of degree of polymerization 30-60 when completing from carboxylate degree of polymerization 3-4 to precondensation，In upper room, intrinsic viscosity is that the melt of 0.1-0.2dl/g was transported in lower room through bosom compartment communicating pipe，Under agitation，Carry out the prepolymerization reaction of the degree of depth，Intrinsic viscosity is promoted to 0.2-0.35dl/g，In overall precondensation process，Not only achieve the significantly lifting of intrinsic viscosity，Be conducive to the optimization of the serviceabilities such as subsequent product machinery，And course of reaction is more terse，Reaction stability is good，The poly-melt of the final final minification obtained，Intrinsic viscosity reaches 0.68dl/g，End carboxyl 20mol/t，Diethylene glycol mass fraction 0.95%，Form and aspect b value less than 2.0.
Accompanying drawing explanation
Fig. 1 is the structural representation of the present invention；
Fig. 2 goes up room perspective view in precondensation still in the present invention；
The top view of Fig. 3 Fig. 2；
Fig. 4 is the structural representation of Dropbox in squirrel-cage agitator in present invention polycondensation vessel at end.
Number in the figure: 1. esterifying kettle one；11. kettle；12. sleeve；13. coil pipe one；14. through hole；15. leg；2. esterifying kettle two；21. mistress；22. interior room；23. coil pipe two；3. precondensation still；31. upper room；32. helical baffle；33. coil pipe three；34. communicating pipe；35. lower room；36. coil pipe four；4. whole polycondensation vessel；41. squirrel-cage agitator one；42. squirrel-cage agitator two；43. Dropbox；431. housing；432. net bar；433. mesh；434. internal ring；44. whole polycondensation vessel framework；45. rotating shaft；51. agitator one；52. agitator two；53. agitator three；6. connecting tube one；7. connecting tube two；8. connecting tube three；9. thermometer.
Detailed description of the invention
Embodiment 1
The present embodiment four still polyplant, in conjunction with Fig. 1, including esterifying kettle 1, esterifying kettle 22, precondensation still 3 and whole polycondensation vessel 4, esterifying kettle 1 is made up of kettle 11, the sleeve 12 being arranged in kettle 11 and coil pipe 1, coil pipe 1 extends from the bottom up of kettle 11 and is surrounded between sleeve 12 and kettle 11, arranging multiple through hole 14 on sleeve 12 wall, kettle 11 is connected by through hole 14 with sleeve 12, arranges agitator 1 in sleeve 12；Esterifying kettle 22 is made up of mistress 21, interior room 22 and the coil pipe 2 23 that is arranged in interior room 22, in conjunction with Fig. 2 and Fig. 3, bottom mistress 21 and interior room 22 obstructed, interior room 22 sidewall arranges hole, mistress 21 is connected by hole with interior room 22, it is provided with support bar between mistress 21 and interior room 22, to support interior room 22 cylinder, interior room 22 arranges agitator 2 52；Precondensation still 3 is vertical structure, including upper room 31 and lower room 35, upper room 31 is obstructed with lower room 35, and upper room 31 is divided into multiple annular compartment by helical baffle 32, arranges coil pipe 3 33 in compartment, the compartment place in bosom, upper room 31 is provided with communicating pipe 34, melt in upper room 31, through sending into lower room 35 communicating pipe 34, arranges thermometer 9, is provided with agitator 3 53 in precondensation still 3 in this communicating pipe 34, agitator 3 53 is arranged in lower room 35, arranges coil pipe 4 36 in lower room 35；nullWhole polycondensation vessel 4 is by squirrel-cage agitator 1、Squirrel-cage agitator 2 42、Dropbox 43、Whole polycondensation vessel framework 44 and rotating shaft 45 are constituted，Squirrel-cage agitator 1 and squirrel-cage agitator 2 42 are provided with multiple Dropbox 43 being parallel to each other，In whole polycondensation vessel 4，The cross-shaped state of net bar of adjacent two panels Dropbox 43，To improve Surface Renewal efficiency during stirring，In conjunction with Fig. 4，Dropbox 43 is by housing 431、Net bar 432、Mesh 433 and internal ring 434 are constituted，Internal ring 434 is arranged with housing 431 concentric，Net bar 432 is crisscross arranged between housing 431 and internal ring 434，Staggered net bar 432 forms mesh 433，Internal ring 434 is set in rotating shaft 45，Dropbox 43 is installed in whole polycondensation vessel framework 44 by rotating shaft 45，In squirrel-cage agitator 1, Dropbox distribution density is big compared with Dropbox distribution density in squirrel-cage agitator 2 42；The material inlet of esterifying kettle 1 is positioned at kettle top, the bottom of esterifying kettle 1 is communicated in the middle part of the mistress 31 of esterifying kettle 22 by connecting tube 1, the bottom of esterifying kettle 22 is communicated in the compartment that on precondensation still, in room 31, outermost layer helical baffle 32 is formed by connecting tube 27, connect connecting tube 38 bottom precondensation still 3 and be communicated to squirrel-cage agitator 1 bottom of whole polycondensation vessel 4, and discharge material through the bottom of squirrel-cage agitator 2 42.
Raw material p-phthalic acid and ethylene glycol it is proportionally added into catalyst and is configured to slurry, esterifying kettle 1 top adding, wherein, esterifying kettle 1 is back-mixing still, coil pipe 1, for going with each other all the time, is from bottom to top disposed with five groups, and first group is two-layer, second group is three layers, 3rd group is four layers, and the 4th group is five layers, and the 5th group is six layers, totally two ten layers, often the spacing between group coil pipe one is 10cm；Slurry enters after in still, agitator 1 is pressed downward against, slurry via through holes 14 circulates back and forth between sleeve 12 and kettle 11, control pressure 52-60kPa, temperature 256-265 DEG C, liquid level 40-70%, carrying out first stage esterification 4 hours, carboxylate is drained in the mistress 21 of esterifying kettle 22 by bottom esterifying kettle 1.
In esterifying kettle 22, coil pipe 2 23 layered laminate arranges and arranges ten groups, room 22 in carboxylate hole entrance on interior room 22, control pressure 2-5kPa, temperature 266-270 DEG C, liquid level 45-70%, in 1.5-2 hour response time, completes the carboxylate after second stage esterification and is delivered in the upper room 31 of precondensation still 3.
In precondensation still 3, in upper room 31, helical baffle 32 is provided with 3 circles, helical baffle 32 is provided with agnail plate, to increase the mixed effect in fluid formation circulation process, nine layers of coil pipe 3 33 it are provided with between helical baffle 32, material enters from an outmost annular compartment, flow in the shape of a spiral, in control, in room 31, temperature is 276-277 DEG C, adopt bubble liquid level meter, liquid level 55-60%, pressure 8.8-9kPa, after material circulates and stops 1 hour in the compartment that helical baffle is formed, enter lower room 35 communicating pipe 34 in innermost layer compartment, and only thermometer is set on the pipeline of upper room material inlet, it is not provided with thermometer in upper room 31；In lower room 35, coil pipe goes with each other all the time, and with layered laminate spread configuration six layers, temperature be 277-278 DEG C, pressure be 1.7kPa, in lower room 35, liquidometer adopts radioactive source liquidometer, when liquid level is 30-45%, stops 1 hour, completing prepolymerization reaction, the prepolycondensate intrinsic viscosity that prepolymerization reaction obtains is 0.20-0.35dl/g.
This prepolycondensate is sent in whole polycondensation vessel 4, controls temperature 275-285 DEG C, liquid level: feed zone (i.e. one 41 sections of squirrel-cage agitator) 60%-90%, discharging section (i.e. 2 42 sections of squirrel-cage agitator) 10%-40%, pressure 100-150Pa, it is thus achieved that whole polycondensation product.
Adopt the four still polyplants of the present embodiment, reactor total quantity reduces, installation footprint reduces, kettle used only needs esterifying kettle 1, esterifying kettle 22, precondensation still 3 and whole 4 four stills of polycondensation vessel, precondensation still 3 therein adopts upper room 31, the mutual disconnected vertical structure in lower room 35, this structure makes equipment integral installation area reduce 1/5, and heating agent makes consumption also be controlled, and integral production cost can reduce 30-50%；nullAnd when adopting this four still polyplants to be polymerized，When carboxylate enters into precondensation stage，It is introduced in the compartment in room 31，In this compartment，Carboxylate is circulated conveying along specific track，The process of conveying completes the initial reaction of precondensation，And achieve the lifting of degree of polymerization 30-60 when completing from carboxylate degree of polymerization 3-4 to precondensation，In upper room 31, intrinsic viscosity is that the melt of 0.1-0.2dl/g is through being transported in lower room 35 bosom compartment communicating pipe 34，Under agitation，Carry out the prepolymerization reaction of the degree of depth，Intrinsic viscosity is promoted to 0.2-0.35dl/g，In overall precondensation process，Not only achieve the significantly lifting of intrinsic viscosity，Be conducive to the optimization of the serviceabilities such as subsequent product machinery，And course of reaction is more terse，Reaction stability is good，The poly-melt of the final final minification obtained，Intrinsic viscosity reaches 0.68dl/g，End carboxyl 20mol/t，Diethylene glycol mass fraction 0.95%，Form and aspect b value less than 2.0.
Therefore, when the above-mentioned four still polyplants adopting the present embodiment are polymerized, the efficiency of package unit improves, handling promotes, can realizing single covering device and produce the Large Copacity device of 500,000 tons of polyester, whole process reaction time decreased per year, device efficiency promotes, simultaneous reactions still quantity reduces, and operation site is reduced.
Embodiment 2
The present embodiment four still polyplant, in conjunction with Fig. 1, including esterifying kettle 1, esterifying kettle 22, precondensation still 3 and whole polycondensation vessel 4, esterifying kettle 1 is made up of kettle 11, the sleeve 12 being arranged in kettle 11 and coil pipe 1, coil pipe 1 extends from the bottom up of kettle 11 and is surrounded between sleeve 12 and kettle 11, arranging multiple through hole 14 on sleeve 12 wall, kettle 11 is connected by through hole 14 with sleeve 12, arranges agitator 1 in sleeve 12；Esterifying kettle 22 is made up of mistress 21, interior room 22 and the coil pipe 2 23 that is arranged in interior room 22, in conjunction with Fig. 2 and Fig. 3, bottom mistress 21 and interior room 22 obstructed, interior room 22 sidewall arranges hole, mistress 21 is connected by hole with interior room 22, it is provided with support bar between mistress 21 and interior room 22, to support interior room 22 cylinder, interior room 22 arranges agitator 2 52；Precondensation still 3 is vertical structure, including upper room 31 and lower room 35, upper room 31 is obstructed with lower room 35, and upper room 31 is divided into multiple annular compartment by helical baffle 32, arranges coil pipe 3 33 in compartment, the compartment place in bosom, upper room 31 is provided with communicating pipe 34, melt in upper room 31, through sending into lower room 35 communicating pipe 34, arranges thermometer 9, is provided with agitator 3 53 in precondensation still 3 in this communicating pipe 34, agitator 3 53 is arranged in lower room 35, arranges coil pipe 4 36 in lower room 35；nullWhole polycondensation vessel 4 is by squirrel-cage agitator 1、Squirrel-cage agitator 2 42、Dropbox 43、Whole polycondensation vessel framework 44 and rotating shaft 45 are constituted，Squirrel-cage agitator 1 and squirrel-cage agitator 2 42 are provided with multiple Dropbox 43 being parallel to each other，In whole polycondensation vessel 4，The cross-shaped state of net bar of adjacent two panels Dropbox 43，To improve Surface Renewal efficiency during stirring，In conjunction with Fig. 4，Dropbox 43 is by housing 431、Net bar 432、Mesh 433 and internal ring 434 are constituted，Internal ring 434 is arranged with housing 431 concentric，Net bar 432 is crisscross arranged between housing 431 and internal ring 434，Staggered net bar 432 forms mesh 433，Internal ring 434 is set in rotating shaft 45，Dropbox 43 is installed in whole polycondensation vessel framework 44 by rotating shaft 45，In squirrel-cage agitator 1, Dropbox distribution density is big compared with Dropbox distribution density in squirrel-cage agitator 2 42；The material inlet of esterifying kettle 1 is positioned at kettle top, the bottom of esterifying kettle 1 is communicated in the middle part of the mistress 31 of esterifying kettle 22 by connecting tube 1, the bottom of esterifying kettle 22 is communicated in the compartment that on precondensation still, in room 31, outermost layer helical baffle 32 is formed by connecting tube 27, connect connecting tube 38 bottom precondensation still 3 and be communicated to squirrel-cage agitator 1 bottom of whole polycondensation vessel 4, and discharge material through the bottom of squirrel-cage agitator 2 42.
Raw material p-phthalic acid and ethylene glycol it is proportionally added into catalyst and is configured to slurry, esterifying kettle 1 top adding, wherein, esterifying kettle 1 is back-mixing still, coil pipe 1, for going with each other all the time, is from bottom to top disposed with five groups, and first group is two-layer, second group is three layers, 3rd group is four layers, and the 4th group is five layers, and the 5th group is six layers, totally two ten layers, often the spacing between group coil pipe one is 40cm；Slurry enters after in still, agitator 1 is pressed downward against, slurry via through holes 14 circulates back and forth between sleeve 12 and kettle 11, control pressure 55-68kPa, temperature 255-260 DEG C, liquid level 40-60%, carrying out first stage esterification 5 hours, carboxylate is drained in the mistress 21 of esterifying kettle 22 by bottom esterifying kettle 1.
In esterifying kettle 22, coil pipe 2 23 layered laminate arranges and arranges ten groups, room 22 in carboxylate hole entrance on interior room 22, control pressure 2-3kPa, temperature 266-270 DEG C, liquid level 45-55%, in 1.5 hours response time, completes the carboxylate after second stage esterification and is delivered in the upper room 31 of precondensation still 3.
In precondensation still 3, in upper room 31, helical baffle 32 is provided with 3 circles, helical baffle 32 is provided with agnail plate, to increase the mixed effect in fluid formation circulation process, nine layers of coil pipe 3 33 it are provided with between helical baffle 32, material enters from an outmost annular compartment, flow in the shape of a spiral, in control, in room 31, temperature is 266-276 DEG C, adopt bubble liquid level meter, liquid level 45-55%, pressure 8.8-9kPa, after material circulates and stops 2 hours in the compartment that helical baffle is formed, enter lower room 35 communicating pipe 34 in innermost layer compartment, and only thermometer is set on the pipeline of upper room material inlet, it is not provided with thermometer in upper room 31；In lower room 35, coil pipe goes with each other all the time, and with layered laminate spread configuration six layers, temperature be 280-285 DEG C, pressure be 2.5kPa, in lower room 35, liquidometer adopts radioactive source liquidometer, when liquid level is 45-55%, stop 1 hour, complete prepolymerization reaction and obtain prepolycondensate.
This prepolycondensate is sent in whole polycondensation vessel 4, controls temperature 280-282 DEG C, liquid level: feed zone (i.e. one 41 sections of squirrel-cage agitator) 70%-80%, discharging section (i.e. 2 42 sections of squirrel-cage agitator) 20%-30%, pressure 120-130Pa, it is thus achieved that whole polycondensation product.
Adopt the four still polyplants of the present embodiment, reactor total quantity reduces, installation footprint reduces, kettle used only needs esterifying kettle 1, esterifying kettle 22, precondensation still 3 and whole 4 four stills of polycondensation vessel, precondensation still 3 therein adopts upper room 31, the mutual disconnected vertical structure in lower room 35, this structure makes equipment integral installation area reduce 1/5, and heating agent makes consumption also be controlled, and integral production cost can reduce 30-50%；nullAnd when adopting this four still polyplants to be polymerized，When carboxylate enters into precondensation stage，It is introduced in the compartment in room 31，In this compartment，Carboxylate is circulated conveying along specific track，The process of conveying completes the initial reaction of precondensation，And achieve the lifting of degree of polymerization 30-60 when completing from carboxylate degree of polymerization 3-4 to precondensation，In upper room 31, intrinsic viscosity is that the melt of 0.1-0.2dl/g is through being transported in lower room 35 bosom compartment communicating pipe 34，Under agitation，Carry out the prepolymerization reaction of the degree of depth，Intrinsic viscosity is promoted to 0.2-0.35dl/g，In overall precondensation process，Not only achieve the significantly lifting of intrinsic viscosity，Be conducive to the optimization of the serviceabilities such as subsequent product machinery，And course of reaction is more terse，Reaction stability is good，The poly-melt of the final final minification obtained，Intrinsic viscosity reaches 0.70dl/g，End carboxyl 24mol/t，Diethylene glycol mass fraction 0.93%，Form and aspect b value less than 2.0.
Therefore, when the above-mentioned four still polyplants adopting the present embodiment are polymerized, the efficiency of package unit improves, handling promotes, can realizing single covering device and produce the Large Copacity device of 500,000 tons of polyester, whole process reaction time decreased per year, device efficiency promotes, simultaneous reactions still quantity reduces, and operation site is reduced.
Comparative example 1: five still polymerization process (reaction pressure is absolute pressure)
Five autoclaves process adopts low mole prop0rtion [n (EG): n (PTA)=1.10-1.20:1].It is esterified 1 still reaction temperature 255-265 DEG C, reaction pressure 170-210kPa, response time 4h, esterification yield 92%；It is esterified 2 still reaction temperature 265-275 DEG C, reaction pressure 50-105kPa, 1.5 hours response time, esterification yield 96%；Precondensation still reaction temperature 270-275 DEG C, reaction pressure 6-25kPa, 0.7-1.5 hour response time；Polycondensation 1 still reaction temperature 275-285 DEG C, reaction pressure 0.6-10kPa, 0.7-1.5 hour response time；Polycondensation 2 still reaction temperature 275-285 DEG C, reaction pressure 0.1kPa, 1.5-3 hour response time；Final products intrinsic viscosity 0.682dl/g, end carboxyl 26mol/t, diethylene glycol content 1.08%, colour b=3.0.Total reaction time needs more than 9 hours, it is necessary to the site of control is many.
Comparative example 2: Du Pont three still flow process (reaction pressure is absolute pressure)
Du Pont three still flow process adopts high molar ratio [n (EG): n (PTA)=1.80-2.00:1], high temperature, fine vacuum reaction condition.Esterifying kettle reaction temperature is 280-305 DEG C, reaction pressure 110kPa, and the response time is 1.5 hours, and esterification yield is 92%；Polycondensation 1 still reaction temperature is 280-285 DEG C, and in 1.0-1.5 hour response time, reaction pressure asks 1.3-2.0kPa；Polycondensation 2 still reaction temperature is 289-290 DEG C, and reaction pressure is 0.27-0.33kPa, 1.0 hours response time.Final products intrinsic viscosity 0.675dl/g, end carboxyl 28mol/t, diethylene glycol content 1.15%, colour 3.4.Total reaction time more than 6 hours, product colour is higher, and diethylene glycol content is high.
Compared with comparative example 1 by embodiment 1, embodiment 2 and can be seen that, in the common five still polymerization methodses that comparative example 1 adopts, need to be equipped with esterifying kettle one, esterifying kettle two, precondensation still one, precondensation still two, whole polycondensation vessel totally five kettlies, the installation in one line of these kettlies, not only floor space is big, and in installation process, it is necessary to it is equipped with substantial amounts of connecting tube, circuit and corresponding heating agent；And in the present invention, kettle used only needs esterifying kettle one, esterifying kettle two, precondensation still and whole four stills of polycondensation vessel, precondensation still therein adopts upper and lower mutual disconnected vertical structure, and this structure makes equipment integral installation area reduce 1/5 on the one hand；On the other hand, also achieve the significantly lifting of intrinsic viscosity, be conducive to the optimization of the serviceabilities such as subsequent product machinery, and course of reaction is more terse, reaction stability is good, the poly-melt of the final final minification obtained, intrinsic viscosity reaches 0.68dl/g, end carboxyl 20mol/t, diethylene glycol mass fraction 0.95%, form and aspect b value less than 2.0.
By embodiment 1, embodiment 2 compares with comparative example 2 and can be seen that, although the three still polymerization process that comparative example 2 adopts decrease the quantity of kettle, but course of reaction needs high temperature, high vacuum condition, reaction is comparatively harsh, course of reaction needs consume substantial amounts of heat energy to maintain the carrying out of reaction, and the heating agent of the present invention uses and measures control, integral production cost can reduce 30-50%, its four still polyplant whole efficiency provided improve, handling promotes, single covering device vast capacity can be realized produce, whole process reaction time decreased, device efficiency promotes, simultaneous reactions still quantity reduces, operation site is reduced.
Above content is the further description provided technical scheme made in conjunction with the preferred embodiment of the present invention; it cannot be assumed that the present invention is embodied as being confined to these explanations above-mentioned; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (5)
1. four still polyplant, it is characterized in that: include esterifying kettle one, esterifying kettle two, precondensation still and whole polycondensation vessel, described esterifying kettle one is made up of kettle, the sleeve being arranged in kettle and coil pipe one, coil pipe one extends from the bottom up of kettle and is surrounded between sleeve and kettle, sleeve wall arranges multiple through hole, kettle is connected by through hole with sleeve, arranges agitator one in sleeve；Described esterifying kettle two is made up of mistress, interior room and the coil pipe two that is arranged in interior room, obstructed bottom mistress and interior room, and interior room sidewall arranges hole, mistress is connected by hole with interior room, it is provided with support bar between mistress and interior room, to support interior room cylinder, interior room arranges agitator two；Described precondensation still is vertical structure, including upper room and lower room, upper room is obstructed with lower room, and described upper room is divided into multiple annular compartment by helical baffle, arranges coil pipe three in compartment, the compartment place in bosom, upper room is provided with communicating pipe, melt in upper room, through sending into lower room communicating pipe, arranges thermometer, is provided with agitator three in precondensation still in this communicating pipe, agitator three is arranged in lower room, arranges coil pipe four in lower room；Described whole polycondensation vessel is made up of squirrel-cage agitator one and squirrel-cage agitator two, it is provided with multiple Dropbox being parallel to each other at squirrel-cage agitator one and squirrel-cage agitator two, and in squirrel-cage agitator one, Dropbox distribution density is big compared with Dropbox distribution density in squirrel-cage agitator two；The material inlet of esterifying kettle one is positioned at kettle top, the bottom of esterifying kettle one is communicated in the middle part of the mistress of esterifying kettle two by connecting tube one, the bottom of esterifying kettle two is communicated in the compartment that on precondensation still, in room, outermost layer helical baffle is formed by connecting tube two, precondensation bottom portion passes through connecting tube tee joint squirrel-cage agitator one bottom to whole polycondensation vessel, and discharges material through the bottom of squirrel-cage agitator two；In described esterifying kettle one, coil pipe one, for going with each other all the time, is from bottom to top disposed with five groups, and first group is two-layer, and second group is three layers, and the 3rd group is four layers, and the 4th group is five layers, and the 5th group is six layers, totally two ten layers；In described esterifying kettle two, coil pipe two is provided with ten groups, and arranges with layered laminate.
2. four still polyplants as claimed in claim 1, it is characterised in that: described upper room adopts bubble liquid level meter to carry out level gauging, and lower room adopts radioactive source liquidometer to carry out level gauging.
3. four still polyplants as claimed in claim 1, it is characterised in that: in described precondensation still, dividing plate is set to 2-8 circle, and dividing plate is provided with agnail plate.
4. four still polyplants as claimed in claim 1, it is characterised in that: described Dropbox is made up of housing, net bar, mesh and internal ring, and internal ring is arranged with housing concentric, and net bar is crisscross arranged between housing and internal ring, and staggered net bar forms mesh.
5. four still polyplants as claimed in claim 4, it is characterised in that: in described whole polycondensation vessel, the cross-shaped state of net bar of adjacent two panels Dropbox.
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Effective date of registration: 20180625 Address after: 312000 2 Wang Hai Road, Doumen Town, Doumen, Shaoxing, Zhejiang Patentee after: ZHEJIANG GUQIANDAO GREEN FIBER CO., LTD. Address before: 312000 Yue Dong Road, Shaoxing, Shaoxing, Zhejiang Province Co-patentee before: ZHEJIANG GUQIANDAO GREEN FIBER CO., LTD. Patentee before: Zhejiang Guxiandao Industrial Fiber Co., Ltd. |