CN202898291U - PBT (polybutylece terephthalate) esterification device - Google Patents
PBT (polybutylece terephthalate) esterification device Download PDFInfo
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- CN202898291U CN202898291U CN201220493767.9U CN201220493767U CN202898291U CN 202898291 U CN202898291 U CN 202898291U CN 201220493767 U CN201220493767 U CN 201220493767U CN 202898291 U CN202898291 U CN 202898291U
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Abstract
The utility model discloses a PBT (polybutylece terephthalate) esterification device, which comprises a reaction kettle and a rectification separating device, wherein the reaction kettle is divided into an upper section and a lower section, the lower section is an agitating area, the upper section is a non-agitating area, the inner diameter of the agitating area is less than the inner diameter of the non-agitating area, a tubular heat exchanger or a heat exchanger coil is arranged in the agitating area, a guide cylinder is arranged in the non-agitating area, the lower end of the guide cylinder is connected with the agitating area, the upper end of the guide cylinder is located in the agitating area, an overflow area is formed between the wall of the guide cylinder and the wall of the non-agitating area, and the bottom or lower part of the overflow area is provided with an esterified liquid discharge outlet; two layers of agitating blades are arranged in the reaction kettle, the lower agitating blades are inclined blades, which are located in the middle of the tubular heat exchanger or heat exchanger coil, and the upper agitating blade is a disc blade, which is located in the non-agitating area over the guide cylinder. The PBT esterification device has the advantages of less catalyst hydrolysis, high esterification rate and the like.
Description
Technical field
The utility model belongs to the production of polyester field, is specifically related to a kind of polybutylene terephthalate production equipment.
Background technology
Polybutylene terephthalate (PBT) is a kind of important engineering materials, is widely used in the fields such as electronics, electrical equipment, fiber, film.Esterification, polycondensation, final minification three phases are namely experienced in the production of normal employing three-stage process.In the esterification stage, raw material terephthalic acid, 1.4-butyleneglycol (BDO), catalyzer (often adopting tetrabutyl titanate as catalyzer) obtain esterification yield through esterification〉94%, the oligopolymer of the polymerization degree between 3～6 is commonly called as carboxylate.Esterification reaction product enters into polycondensation vessel and further carries out polycondensation, obtains the prepolycondensate of polymerizable medium degree, and the precondensation product enters into final polycondensation reactor, further carries out polycondensation, often adopts the disc type polycondensation reactor.Wherein esterification is the committed step of whole process, and the hydroxyl generation esterification of the carboxyl of deacidification and alcohol generates beyond the water, and the dehydration reaction of BDO also occurs, and catalyzer and the reaction of steeping in water for reconstitution unboiled water solution.Titanate catalyst can be hydrolyzed, thermal degradation reaction generates titanium dioxide and other polymer dirt sample compound, sticks to the surface of equipment, and impact is conducted heat, and also can enter into product stream simultaneously, affects quality product.Fouling mainly occurs in the gas-phase space on surface and the reactor top of interchanger.There is no at present more effective catalyzer and substitute tetrabutyl titanate, therefore need a kind of PBT esterification production equipment that can reduce fouling of exploitation.Secondly high esterification yield is the assurance that high quality product is carried out, obtained in the polycondensation of assurance product smoothly.
Summary of the invention
The purpose of this utility model is for the hydrolysis that reduces catalyzer and improves esterification yield, provides a kind of PBT production to use esterification device.
The technical solution of the utility model is:
A kind of PBT esterification device, comprise reactor and rectifying separation device, the vapor outlet port at described reactor top communicates with the gas inlet of rectifying separation device, and the bottom liquid outlet of rectifying separation device communicates with the phegma entrance of reactor top and bottom respectively; Described reactor is divided into two sections, hypomere is stirring area, epimere is non-stirring area, the internal diameter of described stirring area is provided with tubulation heat-exchanger rig or heat exchange coil less than the internal diameter of non-stirring area in stirring area, be provided with guide shell in non-stirring area, the lower end of described guide shell is connected with stirring area, the upper end of guide shell is positioned at stirring area, forms flooded zonevvv between water conservancy diversion barrel and the non-stirring area wall, is provided with the esterifying liquid discharge port in bottom or the bottom of flooded zonevvv; Be provided with the double-deck stirring rake that stirs in reactor, the stirring rake of bottom is tiltedly to starch, and it is positioned at the middle part of described tubulation heat-exchanger rig or heat exchange coil, and the stirring rake on top is the disk oar, and this disk oar is positioned at the guide shell top of non-stirring area.
The phegma entrance at reactor top is located at the top of described disk oar, and perhaps the phegma entrance at described reactor top leads to the top of described disk oar by conduit.The liquid that rectifier unit returns is guided to the top of disk by phegma entrance or conduit, the disk of rotation is thrown to liquid on the still wall.The water that esterification produces and the Tetrahydrofuran of butyleneglycol and generation, in non-stirring area evaporation, the containing on the wall that catalyst reaction liquid can stick to reactor of evaporation, the butyleneglycol liquid of being dished out by the disk oar cleans, and turns back in the reactor.
Described oblique slurry can adopt the oblique oar of 3-6 leaf, and the oblique oar of still bottom produces the cycling stream of large flux, increases the speed of streams through between tubulation or coil pipe, reduces fouling.
The main body of stirring area and non-stirring area is respectively cylindrical, is provided with transition section between between stirring area and the non-stirring area.Stirring area is 1:1.05～1.6 with the diameter ratio of non-stirring area.
The guide shell of reaction zone inside, top, can make the moving esterifying liquid of upwelling overflow to zone between guide shell and the still wall from the top of guide shell, namely in the flooded zonevvv, discharge nozzle is arranged on bottom or the bottom of flooded zonevvv, esterifying liquid flows by the plug flow that rises and descend, and guarantees high esterification yield.
The tubulation heat-exchanger rig is annular, and described oblique slurry is arranged in the middle flow chamber of circumferential alignment tube heat-exchanger.In annular tubulation heat-exchanger rig, the internal diameter of ring is 0.2～0.8:1 with the ratio of external diameter.
Be provided with terephthalic acid and butyleneglycol slurry entrance in the bottom of non-stirring area or at transition section, this entrance leads to described tubulation heat-exchanger rig or the middle top of heat exchange coil by conduit.The conduit segment distance that extends internally from the slurry ingress, and turn to downwards.The esterifying liquid discharge port of described flooded zonevvv can be located at the middle and lower part of transition section.
Terephthalic acid and butyleneglycol are made into slurry according to required ratio, be transported in the reaction kettle of the esterification through mashing pump, in reactor, carry out esterification, water, tetrahydrofuran (THF), part 1 that reaction generates, the 4-butyleneglycol enters in the dehydration tower and dewaters, water is discharged from cat head, and tetrahydrofuran (THF) enters the tetrahydrofuran (THF) recovery tower and reclaims tetrahydrofuran (THF).1, the 4-butyleneglycol is divided into two portions, a part enters reactor with live catalyst from the bottom of reactor, another part enters reactor from the top of reactor, throw the wall of lower reactor through liquid throwing plate, wash away because of the catalyzer on the evaporation adhesive reaction still wall, turn back in the main flow of reactor.
The slurry that enters reactor forms cycling stream in the bottom under the effect of press-down type stirring rake (being oblique oar), esterification mainly occurs in the bottom, the esterification portion of product of bottom, mode with approximate plug flow moves upward, can guarantee high esterification yield (〉 96%), improve follow-up condensation polymerization speed, improve the quality of products.
Device of the present utility model reduces the hydrolysis of catalyzer on the one hand, improves the utilization ratio of catalyzer, improves the quality of products; Reactor is divided into two different chamber on the other hand, can obtain high esterification yield, has improved follow-up condensation polymerization speed, improves the quality of products.
Description of drawings
Fig. 1 is a kind of structural representation of the present utility model.
Among the figure, the 1-reactor, 2-annular tubulation heat exchanging pipe, 3-disk oar, 4-tiltedly starches, 5-agitator motor, 6-feed-pipe, 7-rectifying tower, 8-interchanger, 9-interchanger, 10-lime set tank, 11-guide shell.
The F1-slurry, F2-catalyzer, the gas of F3-evaporation, F4-tower reactor top phegma, F5-tower reactor bottom phegma, F7-cat head lime set refluxes, and F8-cat head lime set is discharged, and F9-cat head non-condensable gases is discharged, the discharging of F10-esterifying liquid, the F11-heating agent advances, and the F12-heating agent goes out.
Embodiment
Below in conjunction with drawings and Examples the utility model is further described.
As shown in Figure 1, the PBT esterification device mainly is comprised of reactor and rectifying separation device two portions.The rectifying separation device comprises rectifying tower 7, interchanger (8,9) and lime set tank 10, the vapor outlet port at esterifier 1 top communicates with the gas inlet of rectifying tower 7, and the bottom liquid outlet of rectifying tower 7 communicates with the phegma entrance of esterifier 1 top and bottom respectively; The pneumatic outlet at rectifying tower 7 tops connects lime set tank 10 by an interchanger 8, and interchanger 8 links to each other with another interchanger 9, and interchanger 9 has the non-condensable gases relief outlet and is back to the condensate port of lime set tank 10.
Be provided with annular tubulation heat exchanging pipe 2 in stirring area, the internal diameter of ring is 0.2～0.8:1 with the ratio of external diameter.Be provided with guide shell 11 in non-stirring area, the lower end of guide shell 11 is connected with stirring area, and the upper end of guide shell 11 is positioned at stirring area, forms flooded zonevvv between water conservancy diversion barrel and the non-stirring area wall.
In reactor 1, be provided with the Double-layer stirring paddle that is driven by agitator motor 5, the stirring rake of bottom is tiltedly slurry 4 of 3-6 leaf, it is arranged in the middle flow chamber of annular tubulation heat exchanging pipe 2, and the stirring rake on top is disk oar 3, and this disk oar 3 is positioned at guide shell 11 tops of non-stirring area.
The phegma entrance at reactor top is located at the top of described disk oar 3, and perhaps the phegma entrance at reactor top leads to the top of described disk oar 3 by conduit.Be provided with terephthalic acid and butyleneglycol slurry entrance in the bottom of non-stirring area or at transition section, this entrance leads to the top of annular tubulation heat exchanging pipe 2 centres by feed-pipe 6.Feed-pipe 6 segment distance that extends internally from the slurry ingress, and turn to downwards.Be provided with the esterifying liquid discharge port in the bottom of flooded zonevvv or the transition section middle and lower part of bottom.On the stirring area wall, also be provided with heating agent import and heating agent outlet for annular tubulation heat exchanging pipe 2.
Terephthalic acid and butyleneglycol slurry F1 are from feed-pipe 6 and inner extension tube, enter into the central upper of lower reaction zone, under the effect of declivity slurry 4, mix with the esterifying liquid of lower reaction zone, PTA is dissolved in the esterifying liquid, produces high-speed circulating stream, fast by in the annular tubulation heat exchanging pipe 2, carry out heat exchange with the heating agent that flows in the tubulation, esterification occurs.The water of partial esterification liquid and generation moves upward along guide shell 11, overflows to flooded zonevvv from the top of guide shell, and from the middle and lower part discharging pipeline F10 discharging of reactor, this mode has guaranteed that esterifying liquid is plug flow flowing of upper area.The water that esterification produces evaporates at upper area, butyleneglycol and water vapour F3 that evaporation produces enter into dehydration tower, in dehydration tower, dewater, butyleneglycol after the dehydration is divided into two portions, approximately the butyleneglycol F5 of 0.6～1 minute rate enters reactor, catalytic esterification from the bottom of reactor with the fresh catalyzer of adding.Approximately the butyleneglycol F4 of 0-0.4 minute rate enters from the top of reactor, is incorporated on the disk oar 3, and the disk oar that is rotated gets rid of to wall, cleans the steam that rises, and the cleaning evaporation sticks to esterifying liquid and catalyzer on the wall.The steam that rises enters into dehydration tower and dewaters, and at first in interchanger 8 after the heat exchange cooling, gas continues further cooling in water cooler 9 to cat head steam out, and the liquid that cooling obtains enters into holding tank 10.The part cooling fluid is back to the rectifying tower cat head, all the other discharges.The temperature of esterification is between 200-250 ℃, and esterification pressure is in the 10-60kpa(absolute pressure), the residence time, the gained esterification yield was greater than 94% between 60-120min.
Claims (8)
1. PBT esterification device, comprise reactor and rectifying separation device, the vapor outlet port at described reactor top communicates with the gas inlet of rectifying separation device, and the bottom liquid outlet of rectifying separation device communicates with the phegma entrance of reactor top and bottom respectively; It is characterized in that described reactor is divided into two sections, hypomere is stirring area, epimere is non-stirring area, the internal diameter of described stirring area is provided with tubulation heat-exchanger rig or heat exchange coil less than the internal diameter of non-stirring area in stirring area, be provided with guide shell in non-stirring area, the lower end of described guide shell is connected with stirring area, the upper end of guide shell is positioned at stirring area, forms flooded zonevvv between water conservancy diversion barrel and the non-stirring area wall, is provided with the esterifying liquid discharge port in bottom or the bottom of flooded zonevvv; Be provided with the double-deck stirring rake that stirs in reactor, the stirring rake of bottom is tiltedly to starch, and it is positioned at the middle part of described tubulation heat-exchanger rig or heat exchange coil, and the stirring rake on top is the disk oar, and this disk oar is positioned at the guide shell top of non-stirring area.
2. PBT esterification device according to claim 1 is characterized in that the phegma entrance at described reactor top is located at the top of described disk oar, and perhaps the phegma entrance at described reactor top leads to the top of described disk oar by conduit.
3. PBT esterification device according to claim 1 is characterized in that described stirring area and the diameter ratio of non-stirring area are 1:1.05～1.6.
4. according to claim 1 or 3 described PBT esterification devices, it is characterized in that the main body of described stirring area and non-stirring area is respectively cylindrical, between between stirring area and the non-stirring area, be provided with transition section.
5. PBT esterification device according to claim 1 is characterized in that described tubulation heat-exchanger rig is annular, and described oblique slurry is arranged in the middle flow chamber of circumferential alignment tube heat-exchanger.
6. PBT esterification device according to claim 5 is characterized in that in the described annular tubulation heat-exchanger rig, and the internal diameter of ring is 0.2～0.8:1 with the ratio of external diameter.
7. PBT esterification device according to claim 4, it is characterized in that being provided with terephthalic acid and butyleneglycol slurry entrance in the bottom of non-stirring area or at transition section, this entrance leads to described tubulation heat-exchanger rig or the middle top of heat exchange coil by conduit.
8. PBT esterification device according to claim 4 is characterized in that the esterifying liquid discharge port of described flooded zonevvv is located at the middle and lower part of transition section.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201220493767.9U CN202898291U (en) | 2012-09-25 | 2012-09-25 | PBT (polybutylece terephthalate) esterification device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201220493767.9U CN202898291U (en) | 2012-09-25 | 2012-09-25 | PBT (polybutylece terephthalate) esterification device |
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| CN202898291U true CN202898291U (en) | 2013-04-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201220493767.9U Expired - Lifetime CN202898291U (en) | 2012-09-25 | 2012-09-25 | PBT (polybutylece terephthalate) esterification device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437287A (en) * | 2013-09-18 | 2015-03-25 | 郑莹 | Reaction apparatus |
| CN109529753A (en) * | 2019-01-14 | 2019-03-29 | 扬州惠通化工科技股份有限公司 | A kind of PBT esterification system |
| CN114682196A (en) * | 2020-12-31 | 2022-07-01 | 中国石油化工集团公司 | Esterification reaction kettle and application thereof |
-
2012
- 2012-09-25 CN CN201220493767.9U patent/CN202898291U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437287A (en) * | 2013-09-18 | 2015-03-25 | 郑莹 | Reaction apparatus |
| CN109529753A (en) * | 2019-01-14 | 2019-03-29 | 扬州惠通化工科技股份有限公司 | A kind of PBT esterification system |
| CN114682196A (en) * | 2020-12-31 | 2022-07-01 | 中国石油化工集团公司 | Esterification reaction kettle and application thereof |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130424 |