CN111777755A - Final polycondensation reactor for preparing polycarbonate - Google Patents

Final polycondensation reactor for preparing polycarbonate Download PDF

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Publication number
CN111777755A
CN111777755A CN202010630764.4A CN202010630764A CN111777755A CN 111777755 A CN111777755 A CN 111777755A CN 202010630764 A CN202010630764 A CN 202010630764A CN 111777755 A CN111777755 A CN 111777755A
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CN
China
Prior art keywords
disc
shell
feeding
inlet
material passing
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Pending
Application number
CN202010630764.4A
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Chinese (zh)
Inventor
陈超
张雪峰
朱玉成
黄刚
刘国柱
闫卫林
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Lihuayi Weiyuan Chemical Co ltd
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Lihuayi Weiyuan Chemical Co ltd
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Priority to CN202010630764.4A priority Critical patent/CN111777755A/en
Publication of CN111777755A publication Critical patent/CN111777755A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G64/00Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
    • C08G64/20General preparatory processes
    • C08G64/205General preparatory processes characterised by the apparatus used
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/0021Degasification of liquids by bringing the liquid in a thin layer
    • B01D19/0026Degasification of liquids by bringing the liquid in a thin layer in rotating vessels or in vessels containing movable parts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/006Processes utilising sub-atmospheric pressure; Apparatus therefor

Abstract

The invention discloses a final polycondensation reactor for preparing polycarbonate, which comprises a horizontal cylindrical shell, wherein the shell is provided with a feed inlet and a product outlet, the feed inlet is connected with a feed pipeline, a rotary cylinder is arranged in the shell, the front end of the rotary cylinder is provided with an inlet, and the feed pipeline penetrates through the inlet and is inserted into the rotary cylinder; a driving shaft is arranged in the center of the rotary cylinder; the rotary drum is characterized in that a feeding disc is arranged at the front end of the interior of the rotary drum close to an inlet, a discharging disc is arranged at the rear end of the interior of the rotary drum, and a support frame and a plurality of material passing discs are arranged in the middle of the interior of the rotary drum. When the reactor of the invention is operated, the prepolymer melt can completely infiltrate the inner surface of the cylinder and the surface of the material passing disc, so that the phenol removal rate is increased, the reaction rate is increased, excessive polymerization or side reaction caused by part of material viscosity is prevented, the residence time distribution of all prepolymers is narrow, and finally, a polycarbonate product with narrow molecular weight distribution and low impurity content is obtained.

Description

Final polycondensation reactor for preparing polycarbonate
Technical Field
The invention relates to the field of polycarbonate production, in particular to a final polycondensation reactor for preparing polycarbonate.
Background
The final polycondensation reaction of the process for preparing the polycarbonate by the melt transesterification method is an esterification reaction, and the precondensed melt generates micromolecule products of phenol and polycarbonate products under the conditions of high temperature and high vacuum. Phenol needs to be continuously removed in the reaction process, and the mixture is uniformly stirred, so that partial prepolymer is prevented from staying for a long time, excessive polycondensation and yellowing are prevented, and the completion of the polycondensation reaction is promoted.
The final polycondensation reactor is generally a horizontal disc reactor, and inside the disc reactor, a disc rotates to form a melt film, so that the volatilization surface area is increased, the phenol volatilization speed is increased, and the final polycondensation reaction is promoted to be carried out towards the direction of increasing the molecular weight.
However, in the disc reactor, a gap is formed between the disc and the cylinder, high-viscosity melt is easy to remain on the inner side surface and the upper part of the cylinder and cannot be scraped out by the disc, the mass and heat transfer are difficult, the time of the high-viscosity melt stays too long in a high-temperature environment, and partial condensation polymer is excessively condensed to generate side reaction and crystallization. Excessive polycondensation leads the molecular weight distribution of the polycarbonate product to be widened, and the mechanical property of the product is reduced; the side reaction causes yellowing of the product to generate yellow spots and or pock spots, and crystallization causes crystal spots of the product to be generated, thereby reducing the optical performance of the product.
The other falling film or gravity flow reactor has no stirrer, no need of considering dynamic sealing, high vacuum degree and is favorable to phenol volatilization. However, the polycarbonate prepolymer melt flows down along the molded article only by gravity inside the reactor, and due to the high melt viscosity, it remains on a part of the surface and flows unevenly, causing excessive polycondensation, crystallization, and further forming yellow and black spots.
Disclosure of Invention
The invention provides a final polycondensation reactor for preparing polycarbonate, which solves the problems that high-viscosity materials in the existing horizontal disc reactor flow unevenly, the materials stay for a long time and side reactions are easy to occur.
The technical scheme of the invention is as follows: the utility model provides a preparation polycarbonate's final polycondensation reactor, includes horizontal cylinder casing, the casing is equipped with feed inlet and product export, its characterized in that: the feeding end of the shell is provided with a feeding end sealing head, the outlet end of the product is provided with a driving end sealing head, a rotating cylinder body is arranged in the shell, a supporting rod is arranged in the shell and close to the feeding end sealing head, the front end of the rotating cylinder body is provided with an inlet, the inlet is connected with a supporting shaft, the supporting shaft is a hollow shaft, a bearing is sleeved outside the supporting shaft, the outer ring of the bearing is connected with the top of the supporting rod, the feeding port is connected with a feeding pipeline, and the feeding pipeline penetrates through the supporting;
a driving shaft is arranged in the center of the rotating cylinder body, and the rear end of the driving shaft penetrates through the driving end head to be connected with a driving motor; the rotary drum is characterized in that a feeding disc is arranged at the front end of the interior of the rotary drum close to an inlet, a discharging disc is arranged at the rear end of the interior of the rotary drum, a support frame and a plurality of material passing discs are arranged in the middle of the rotary drum, the feeding disc, the discharging disc and the support frame are all inner wall connection driving shafts and outer wall connection rotary drums, the material passing discs are uniformly distributed between the feeding disc and the discharging disc, the outer wall connection rotary drums of the material passing discs are arranged, gaps are reserved between the inner walls of the material passing discs and the driving shafts, the inner diameters of the material passing discs are gradually increased from the feeding disc to the discharging disc, a plurality of through holes are formed in the feeding disc.
Further, the method comprises the following steps of; the driving shaft is connected with the driving end head through a sealing bearing.
Further, the method comprises the following steps of; an annular baffle is arranged in the shell and close to the end seal of the driving end, a gap is reserved between the inner wall of the annular baffle, which is connected with the driving shaft, the outer wall of the annular baffle and the shell, and a product outlet of the shell corresponds to the gap between the annular baffle and the discharge disc.
Further, the method comprises the following steps of; and a convex ring is arranged on the outer wall of the rear end of the rotary cylinder body.
Further, the method comprises the following steps of; the shell is provided with a vacuum connector and a residual liquid outlet, the residual liquid outlet is close to the front end of the rotary cylinder, and the shell is provided with a residual liquid baffle at the product outlet.
Further, the method comprises the following steps of; the number of the rings concentrically distributed in the feeding disc through holes and the discharging disc through holes is 4.
Further, the method comprises the following steps of; the number of the rings concentrically distributed in the through holes of the material passing disk is 3.
Further, the method comprises the following steps of; the heat-conducting oil heat exchanger is characterized in that a heat-conducting oil interlayer is arranged on the inner wall of the shell, a heat-conducting oil inlet and a heat-conducting oil outlet are formed in the heat-conducting oil interlayer, and heat-conducting oil jackets are arranged at the feed inlet, the product outlet, the vacuum connector and the residual liquid outlet of the shell.
The invention has the beneficial effects that: when the reactor of the invention is operated, the prepolymer melt flows in the rotary cylinder body in the radial and longitudinal directions simultaneously under the conditions of high temperature and high vacuum, and a uniform film is formed on the inner surface of the rotary cylinder body and the material passing disc to carry out polycondensation reaction and remove phenol gas phase. The prepolymer melt can completely infiltrate the inner surface of the cylinder and the surface of the material passing disc, so that the phenol removal rate is increased, the reaction rate is increased, excessive polymerization or side reaction caused by part of material viscosity is prevented, the residence time distribution of all prepolymers is narrow, and finally, a polycarbonate product with narrow molecular weight distribution and low impurity content is obtained.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a side view of the feed puck of FIG. 1;
FIG. 3 is a side view of the take-off puck of FIG. 1;
FIG. 4 is a side view of the feed block disk of FIG. 1;
fig. 5 is a side view of the support bracket of fig. 1.
In the figure: 1. a feed inlet; 2. a feed conduit; 3. a heat transfer oil inlet; 4. a feed disc; 5. a housing; 6. rotating the cylinder; 7. a material passing disc; 8. a vacuum interface; 9. a discharge disc; 10. a driving end socket; 11. sealing the bearing; 12. an annular baffle; 13. a drive motor; 14. a drive shaft; 15. a material passing disc through hole; 16. a product outlet; 17. a raffinate baffle; 18. a discharge disc through hole; 19. a heat conducting oil outlet; 20. a support frame; 21. a feed disc through hole; 22. a residual liquid outlet; 23. a support bar; 24. A convex ring; 25. a bearing; 26. a support shaft; 27. and sealing a feed end.
Detailed Description
Example (b):
as shown in fig. 1 to 5, a final polycondensation reactor for preparing polycarbonate comprises a horizontal cylindrical shell 5, wherein the shell 5 is provided with a feed inlet 1 and a product outlet 16, the feed end of the shell 5 is provided with a feed end head 27, the product outlet end is provided with a drive end head 10, and the feed end head 27 and the drive end head 10 are both connected with the shell 5 through bolts, so that the final polycondensation reactor is convenient to disassemble and maintain. Sealing gaskets are arranged between the feed end sealing head 27 and the drive end sealing head 10 and between the shell 5.
A rotary cylinder body 6 is arranged in the shell 5, a support rod 23 is arranged in the shell 5 at a position close to a feed end sealing head 27, an inlet is formed in the front end of the rotary cylinder body 6, the inlet is connected with a support shaft 26, the support shaft 26 is a hollow shaft, a bearing 25 is sleeved outside the support shaft 26, the outer ring of the bearing 25 is connected with the top of the support rod 23, the support rod 23 is used for supporting the rotary cylinder body 6, the feed port 1 is connected with a feed pipeline 2, and the feed pipeline 2 penetrates through the support shaft 26 and is inserted into the rotary cylinder body 6;
a driving shaft 14 is arranged at the center of the rotating cylinder 6, the rear end of the driving shaft 14 penetrates through the driving end head 10 to be connected with a driving motor 13, and the driving shaft 14 is connected with the driving end head 10 through a sealing bearing 11; the rotary drum is characterized in that a feeding disc 4 is arranged at the front end of the interior of the rotary drum 6 close to an inlet, a discharging disc 9 is arranged at the rear end of the interior of the rotary drum, two annular support frames 20 and a plurality of material passing discs 7 are arranged in the middle of the interior of the rotary drum, and the feeding disc 4, the discharging disc 9 and the support frames 20 are all inner wall bolt connection driving shafts 14 and outer wall bolt connection rotary drums 6. The support frame 20 provides support for the inner space of the rotary cylinder 6.
The material passing disc 7 is uniformly distributed between the feeding disc 4 and the discharging disc 9, the outer wall of the material passing disc 7 is connected with the rotary cylinder 6, a gap is reserved between the inner wall of the material passing disc 7 and the driving shaft 14, the inner diameter of the material passing disc 7 is gradually increased from the feeding disc 4 to the discharging disc 9, the feeding disc 4 is provided with a feeding disc through hole 21, the discharging disc 9 is provided with a discharging disc through hole 18, the material passing disc 7 is provided with a material passing disc through hole 15, and the feeding disc through hole 21, the discharging disc through hole 18 and the material passing disc through hole 15 are all distributed concentrically in an annular shape with different diameters. The number of the concentric rings of the feeding disc through holes 21 and the discharging disc through holes 18 is 4, and the number of the concentric rings of the passing disc through holes 15 is 3.
An annular baffle 12 is arranged at the end, close to the driving end seal head 10, in the shell 5, the inner wall of the annular baffle 12 is connected with a driving shaft 14, a gap is reserved between the outer wall of the annular baffle 12 and the shell 5, a product outlet 16 of the shell 5 corresponds to the gap between the annular baffle 12 and the discharging disc 9, and a convex ring 24 is arranged on the outer wall of the rear end of the rotary cylinder 6.
The housing 5 is provided with a vacuum connection 8 and a raffinate outlet 22, the vacuum connection 8 being connected to a vacuum system. The residual liquid outlet 22 is close to the front end of the rotary cylinder 6, the residual liquid outlet 22 is used for recovering a trace amount of melt flowing out from a gap between the feeding pipeline 2 and the supporting shaft 26, and the shell 5 is provided with a residual liquid baffle 17 at the product outlet 16 to prevent residual liquid from flowing into a product.
The inner wall of the shell 5 is provided with a heat conduction oil interlayer, the heat conduction oil interlayer is provided with a heat conduction oil inlet 3 and a heat conduction oil outlet 19, and the feed inlet 1, the product outlet 16, the vacuum connector 8 and the residual liquid outlet 22 of the shell 5 are all provided with heat conduction oil jackets to provide heat for melt and gas phase, maintain a flowing state and prevent the melt and the gas phase from solidifying.
The working principle is as follows: the precondensation melt enters from a reactor feed inlet 1 and flows into the rotary cylinder 6 through an inlet pipeline 2, the rotary cylinder 6 continuously rotates at a certain speed under the drive of a drive motor 13, the precondensation melt has viscosity, the melt at the lower part is taken to the upper part and flows down along the surface of the rotary feed disc 4 under the action of gravity and passes through a feed disc through hole 21 to simultaneously flow in the longitudinal direction and the radial direction, the melt fully infiltrates the inner surface of the rotary cylinder 6 and the surface of the material passing disc 7, and a uniform film is formed on the inner surface of the rotary cylinder 6 and the material passing disc 7. The material passing disk through holes 15 arranged on the material passing disk 7 are beneficial to melt film forming, increase the volatilization surface area, increase the phenol volatilization speed and accelerate the pre-polycondensation reaction.
Along with the polycondensation reaction, the viscosity of the melt is gradually increased, the flow rate is gradually reduced, the melt which is brought to the upper part by the rotation of the rotary cylinder body 6 flows downwards along the passing disc 7, and the inner diameter of the passing disc 7 is gradually increased from the feeding disc 4 to the discharging disc 9, so that the flow path of the melt can be shortened along with the polycondensation reaction, the melt can completely infiltrate the passing disc 7, and the flowing dead angle is prevented.
The product melt flows radially out of the discharge disc through-holes 18 at the bottom of the rotating cylinder 6, and the projecting ring 24 and the annular baffle 12 guide the product melt to flow entirely into the product outlet 16 and finally out of the reactor. The residence time of the melt in the reactor is uniform, the melt can fully infiltrate the inner surface of the rotary cylinder 6 and the surface of the material passing disc 7, the reaction area has no dead angle, partial prepolymer is prevented from excessive polycondensation, and finally, the polycarbonate product with narrow molecular weight distribution and high mechanical property and optical property is obtained.
Micromolecule products such as phenol and the like generated by the polycondensation are volatilized to the upper space, flow out of the rotary cylinder body 6 through the discharge disc through hole 18 and enter a vacuum system through the vacuum interface 8.
The pre-condensed melt also flows through the driving shaft 14 inside the rotating cylinder 6, and because the rotating cylinder 6 rotates, the melt on the driving shaft 14 continuously flows, and a part of the melt does not stay for a long time.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.
In the description of the present invention, it is to be understood that the terms indicating an orientation or positional relationship are based on the orientation or positional relationship shown in the drawings only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.

Claims (8)

1. The utility model provides a preparation polycarbonate's final polycondensation reactor, includes horizontal cylinder casing, the casing is equipped with feed inlet and product export, its characterized in that: the feeding end of the shell is provided with a feeding end sealing head, the outlet end of the product is provided with a driving end sealing head, a rotating cylinder body is arranged in the shell, a supporting rod is arranged in the shell and close to the feeding end sealing head, the front end of the rotating cylinder body is provided with an inlet, the inlet is connected with a supporting shaft, the supporting shaft is a hollow shaft, a bearing is sleeved outside the supporting shaft, the outer ring of the bearing is connected with the top of the supporting rod, the feeding port is connected with a feeding pipeline, and the feeding pipeline penetrates through the supporting;
a driving shaft is arranged in the center of the rotating cylinder body, and the rear end of the driving shaft penetrates through the driving end head to be connected with a driving motor; the rotary drum is characterized in that a feeding disc is arranged at the front end of the interior of the rotary drum close to an inlet, a discharging disc is arranged at the rear end of the interior of the rotary drum, a support frame and a plurality of material passing discs are arranged in the middle of the rotary drum, the feeding disc, the discharging disc and the support frame are all inner wall connection driving shafts and outer wall connection rotary drums, the material passing discs are uniformly distributed between the feeding disc and the discharging disc, the outer wall connection rotary drums of the material passing discs are arranged, gaps are reserved between the inner walls of the material passing discs and the driving shafts, the inner diameters of the material passing discs are gradually increased from the feeding disc to the discharging disc, a plurality of through holes are formed in the feeding disc.
2. The final polycondensation reactor for producing polycarbonate according to claim 1, wherein: the driving shaft is connected with the driving end head through a sealing bearing.
3. The final polycondensation reactor for producing polycarbonate according to claim 1, wherein: an annular baffle is arranged in the shell and close to the end seal of the driving end, a gap is reserved between the inner wall of the annular baffle, which is connected with the driving shaft, the outer wall of the annular baffle and the shell, and a product outlet of the shell corresponds to the gap between the annular baffle and the discharge disc.
4. The final polycondensation reactor for producing polycarbonate according to claim 1, wherein: and a convex ring is arranged on the outer wall of the rear end of the rotary cylinder body.
5. The final polycondensation reactor for producing polycarbonate according to claim 1, wherein: the shell is provided with a vacuum connector and a residual liquid outlet, the residual liquid outlet is close to the front end of the rotary cylinder, and the shell is provided with a residual liquid baffle at the product outlet.
6. The final polycondensation reactor for producing polycarbonate according to claim 1, wherein: the number of the rings concentrically distributed in the feeding disc through holes and the discharging disc through holes is 4.
7. The final polycondensation reactor for producing polycarbonate according to claim 1, wherein: the number of the rings concentrically distributed in the through holes of the material passing disk is 3.
8. The final polycondensation reactor for producing polycarbonate according to claim 1, wherein: the heat-conducting oil heat exchanger is characterized in that a heat-conducting oil interlayer is arranged on the inner wall of the shell, a heat-conducting oil inlet and a heat-conducting oil outlet are formed in the heat-conducting oil interlayer, and heat-conducting oil jackets are arranged at the feed inlet, the product outlet, the vacuum connector and the residual liquid outlet of the shell.
CN202010630764.4A 2020-07-03 2020-07-03 Final polycondensation reactor for preparing polycarbonate Pending CN111777755A (en)

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CN202010630764.4A CN111777755A (en) 2020-07-03 2020-07-03 Final polycondensation reactor for preparing polycarbonate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102021113135A1 (en) 2021-05-20 2022-11-24 ventUP GmbH Horizontal rotating thin film degasser

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10218998A (en) * 1997-02-03 1998-08-18 Mitsubishi Heavy Ind Ltd Production of polycondensation polymer
CN101612546A (en) * 2009-05-27 2009-12-30 中国纺织工业设计院 High-efficiency multi-section type final polycondensation reactor
CN203816607U (en) * 2014-03-06 2014-09-10 无锡市兴盛新材料科技有限公司 Disk reactor for continuous polymerization of PBT (polybutylene terephthalate)
CN104841346A (en) * 2015-04-28 2015-08-19 华东理工大学 Disc reactor for gas desorption of absorbents different in viscosity
CN207614844U (en) * 2017-11-29 2018-07-17 中蓝晨光化工研究设计院有限公司 A kind of horizontal reactor continuously preparing makrolon suitable for ester-interchange method
CN212560069U (en) * 2020-07-03 2021-02-19 利华益维远化学股份有限公司 Final polycondensation reactor for preparing polycarbonate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10218998A (en) * 1997-02-03 1998-08-18 Mitsubishi Heavy Ind Ltd Production of polycondensation polymer
CN101612546A (en) * 2009-05-27 2009-12-30 中国纺织工业设计院 High-efficiency multi-section type final polycondensation reactor
CN203816607U (en) * 2014-03-06 2014-09-10 无锡市兴盛新材料科技有限公司 Disk reactor for continuous polymerization of PBT (polybutylene terephthalate)
CN104841346A (en) * 2015-04-28 2015-08-19 华东理工大学 Disc reactor for gas desorption of absorbents different in viscosity
CN207614844U (en) * 2017-11-29 2018-07-17 中蓝晨光化工研究设计院有限公司 A kind of horizontal reactor continuously preparing makrolon suitable for ester-interchange method
CN212560069U (en) * 2020-07-03 2021-02-19 利华益维远化学股份有限公司 Final polycondensation reactor for preparing polycarbonate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102021113135A1 (en) 2021-05-20 2022-11-24 ventUP GmbH Horizontal rotating thin film degasser

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