CN209530859U - A kind of PBT esterification device - Google Patents

A kind of PBT esterification device Download PDF

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Publication number
CN209530859U
CN209530859U CN201920053188.4U CN201920053188U CN209530859U CN 209530859 U CN209530859 U CN 209530859U CN 201920053188 U CN201920053188 U CN 201920053188U CN 209530859 U CN209530859 U CN 209530859U
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China
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catalyst
esterification
reaction kettle
slurry
outlet
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CN201920053188.4U
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曹文
曾庆
张建纲
张跃胜
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Yangzhou Huitong Technology Co.,Ltd.
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Yangzhou Huitong Chemical Polytron Technologies Inc
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Abstract

The utility model relates to a kind of PBT esterification devices, the top center of reaction kettle of the esterification is equipped with stirring port, the side of stirring port is equipped with slurry import and gaseous phase outlet, the inner cavity of reaction kettle of the esterification is separated into mistress and interior room by ring baffle, the lower central of interior room is equipped with inner cylinder, heating tubulation is distributed in the annulus of inner cylinder periphery, slurry import is plugged with the slurry inside extending tube for protruding into reaction kettle inner cavity, slurry inside extending tube includes the vertical section being linked together from top to bottom, segmental arc and tilting section, the lower port of tilting section is located at right above the inner cavity of inner cylinder and apart from 100~150mm of reaction kettle highest liquid level, the bending radius of slurry inside extending tube segmental arc is six to ten times of slurry inside extending tube internal diameter.The bottom centre of reaction kettle of the esterification is equipped with catalyst inlet, and catalyst inlet is equipped with catalyst rising pouring valve.The device can not only be pumped to avoid slurry in charging, but also can be to avoid slurry pipe blocking or catalyst tube blocking, it is ensured that the continuous and steady operation of production improves product quality.

Description

A kind of PBT esterification device
Technical field
The utility model relates to a kind of PBT production system more particularly to a kind of PBT esterification devices, belong to production of polyester Equipment technical field.
Background technique
Polybutylene terephthalate (PBT) abbreviation PBT, belongs to polyester series, is by 1,4-butanediol (BDO) and to benzene two Formic acid (PTA) or terephthalate (DMT) polycondensation form.
The PBT reaction kettle of the esterification of three kettle processes is collet vertical retort, and inside and outside cell structure, interior room is into raw material, mistress's discharging.It is interior Baffle is equipped between mistress, baffle top is equipped with discharging seam, and carboxylate covers discharging seam minimum point, discharges after a week around mistress.It is interior The lower central of room is equipped with inner cylinder, and the stirrer paddle with esterifying kettle coaxial line is equipped in inner cylinder, and stirrer paddle is mounted on agitating shaft Lower end, the driving end of agitating shaft is stretched out from the stirring port of esterifying kettle top center.The periphery of inner cylinder is equipped with heating tubulation, provides Heat needed for esterification.Esterification is negative reaction, and the top of esterifying kettle is equipped with gaseous phase outlet, slurry import and catalysis Agent import, due to the biggish region of top center that stirring port occupies esterifying kettle, gaseous phase outlet and slurry import can only be arranged In the position for deviateing esterifying kettle top center.
If slurry is directly fallen from slurry import, part size is easy to bring knockout tower by the negative pressure at gaseous phase outlet In, it can not be reacted;Region where remaining slurry alignment heating tubulation is fallen, and can partially be sticked to the shell of heating tubulation On, it is easy to carbonize because of overheat, generates black material.In addition, if slurry pipe is inserted into esterifying kettle directly down from slurry import In liquid Space, after producing a period of time, slurry pipe is easy blocking, causes the interruption of production.
PBT polymerization catalyst is butyl titanate, it meets water capacity facile hydrolysis, loses activity, while generating the water of titanium Object is closed, blocking pipeline is easy, influences the addition of catalyst.Butyl titanate is both catalyst for esterification reaction and polycondensation reaction Catalyst, so will be generally added from esterification stage, but esterification can generate a large amount of water.
Existing catalyst preparation method is to be mixed in preparing tank with a certain amount of catalyst and fresh 1,4- butanediol (BDO) It prepares, finished pot is transferred to after preparing, then be added to esterifying kettle after being mixed by pump conveying with process tower reuse high temperature BDO.This Kind method can prevent prepared catalyst solution room temperature from entering esterifying kettle, meet high-temperature evaporation, but fresh BDO and high temperature suddenly All aqueous in reuse BDO, catalyst has grown easy hydrolysis using the time, blocks pipeline, influences to produce.
Utility model content
The purpose of this utility model is that overcoming problems of the prior art, a kind of PBT esterification device is provided, Not only can be pumped, but also can be blocked to avoid slurry pipe or slurry charing in charging to avoid slurry, it is ensured that production it is continuous steady Fixed operation, improves product quality.
In order to solve the above technical problems, a kind of PBT esterification device of the utility model, including reaction kettle of the esterification, it is described The top center of reaction kettle of the esterification is equipped with stirring port, and the side of the stirring port is equipped with slurry import and gaseous phase outlet, the ester The inner cavity for changing reaction kettle is separated into mistress and interior room by ring baffle, and the lower central of interior room is equipped with inner cylinder, the inner cylinder periphery Annulus in heating tubulation is distributed with, the slurry import is plugged with the slurry inside extending tube for protruding into reaction kettle inner cavity, described Slurry inside extending tube includes the vertical section being linked together from top to bottom, segmental arc and tilting section, and the lower port of the tilting section is located at Right above the inner cavity of the inner cylinder and apart from 100~150mm of reaction kettle highest liquid level, the bending of the slurry inside extending tube segmental arc Radius is six to ten times of slurry inside extending tube internal diameter.
Compared with the existing technology, the utility model achieves following the utility model has the advantages that the bending radius of segmental arc is in slurry Six to ten times for stretching bore, it is ensured that the flowing of fresh slurry is smooth, sluggish or buildup will not occur at turning;Fresh slurry Material is directed to right above the inner cavity of inner cylinder through slurry inside extending tube, it is ensured that whole raw materials each fall within the inner cavity of inner cylinder, in inner cylinder It is stirred until homogeneous with material in kettle, flows downward on one side on one side, heating tubulation is entered after the outflow of the lower edge of inner cylinder, is heated on one side Reaction flows up on one side, and the heat power that heating tubulation is thermally formed maintains Natural Circulation of the material inside and outside inner cylinder.This is practical It is novel do not have fresh slurry and fall on the shell of heating tubulation carbonized because of overheat, the lower port of slurry inside extending tube only distance Reaction kettle highest 100~150mm of liquid level not only can avoid raw material and be pumped because of negative pressure, but also while avoiding high liquid level from producing feeds pipe plug Plug influences production.
As the improvement of the utility model, the reaction kettle of the esterification is up big and down small structure, the lower end of the ring baffle It is welded on the kettle wall of the heating tubulation upper limb, the top of the ring baffle is equipped with discharging seam, with ring baffle root pair The kettle wall answered is equipped with discharge port, and radial partition is equipped between the discharging seam and the discharge port.The PBT of end of reaction is from ring The discharging on shape baffle top, which is stitched, overflows, and the radially barrier of partition, PBT flows after a week along annular groove, flows out from discharge port.
Respectively heating tubulation is vertically extending as a further improvement of the utility model, and penetrates through, where heating tubulation Kettle wall lower part is connected with tubulation Heating medium, and the kettle wall top where heating tubulation is connected with the outlet of tubulation heating agent.Material is along each The tube side of heating tubulation flows up, and heating agent such as conduction oil walks the shell side outside tubulation, and the heating of heating agent makes material shape in pipe At the power flowed up.
The bottom centre of the reaction kettle of the esterification is equipped with catalyst inlet, institute as a further improvement of the utility model, It states catalyst inlet and catalyst rising pouring valve is installed;Barrel pump is built-in in catalyst bucket, the outlet of the barrel pump is defeated by barrel pump Outlet pipe is connected with the feed inlet of catalyst tank, and the air inlet at the top of the catalyst tank is connected with the outlet of nitrogen tube, described to urge The discharge port of agent tank is connected with the entrance of catalyst dosing pump, the outlet of the catalyst dosing pump and catalyst filter Entrance is connected, and the outlet of the catalyst filter is connected with the material inlet of catalyst heater, the catalyst heater Material outlet be connected with the entrance of the catalyst rising pouring valve by catalyst rising pouring pipe.Catalyst butyl titanate sheet as Liquid is easy conveying, and using this characteristic, the butyl titanate in catalyst bucket is sent out by barrel pump, is entered by barrel pump efferent duct It is stored in catalyst tank, the gas-phase space of catalyst tank is filled with the nitrogen from nitrogen tube and protects to catalyst, catalysis Catalyst in agent tank is directly extracted out by catalyst dosing pump and is measured, and is not needed to be prepared with the i.e. BDO of 1,4-butanediol, is simultaneously Prevent catalyst from meeting high-temperature evaporation suddenly, the catalyst that catalyst dosing pump is sent out by catalyst heater is preheating to 120 ~ 170 DEG C be sent into reaction kettle of the esterification in.Since esterification can generate a large amount of water in reaction kettle of the esterification, the density of water is less than PBT's Density;Fresh catalyst is injected by catalyst rising pouring pipe and catalyst rising pouring valve from the bottom of reaction kettle of the esterification, can be to avoid Catalyst is contacted with water.
The Heating medium of the catalyst heater is equipped with steam adjusting as a further improvement of the utility model, The entrance of valve, the steam control valve is connected with steam pipe, and the material outlet of the catalyst heater is equipped with temperature sensing Device, the aperture of the steam control valve are controlled by the catalyst temperature that the temperature sensor measures;The catalyst heater Heating agent outlet be connected with drip pipe.The catalyst temperature of the outlet of the catalyst heater measured by the temperature sensor is high When setting upper limit value, then the aperture of steam control valve becomes smaller;It urges the outlet of the catalyst heater measured by the temperature sensor When agent temperature is lower than preset lower limit, then the aperture of steam control valve increases, and can automatically keep the stabilization of catalyst temperature.
The catalyst bucket is placed on transport trolley as a further improvement of the utility model, the outlet of the barrel pump It is connected by connecting hose with the barrel pump efferent duct, the feed inlet of the catalyst tank is equipped with catalyst tank inlet valve, described The entrance of catalyst tank inlet valve is connected with the barrel pump efferent duct.Transport trolley carries catalyst bucket and reaches barrel pump efferent duct Inlet after being connected using connecting hose, is opened catalyst tank inlet valve, can start barrel pump, to catalyst tank injecting catalyst.
Detailed description of the invention
Utility model will be further described in detail below with reference to the attached drawings and specific embodiments, and attached drawing only provides ginseng It examines and illustrates to use, it is non-to limit the utility model.
Fig. 1 is the main view of reaction kettle of the esterification in the utility model.
Fig. 2 is the cross-sectional view in Fig. 1 at ring baffle.
Fig. 3 is the cross-sectional view heated at tubulation in Fig. 1.
Fig. 4 is the flow chart of the utility model PBT esterification device.
In figure: 1. reaction kettle of the esterification;1a. slurry import;1b. gaseous phase outlet;1c. stirring port;1d. discharge port;1e. catalysis Agent entrance;1f. slurry inside extending tube;1g. ring baffle;1g1. discharging seam;1g2. radial direction partition;1h. heats tubulation;1j. tubulation Heating medium;The outlet of 1k. tubulation heating agent;1m. evacuation port;1n. inner cylinder;2. catalyst tank;3. catalyst dosing pump;4. catalyst Filter;5. catalyst heater;6. catalyst bucket;7. transport trolley;G1. barrel pump efferent duct;G2. nitrogen tube;G3. steam Pipe;G4. catalyst rising pouring pipe;G5. drip pipe;V1. catalyst tank inlet valve;V2. catalyst rising pouring valve;V3. steam Regulating valve;T1. temperature sensor.
Specific embodiment
As shown in Figure 1, the PBT esterification device of the utility model includes reaction kettle of the esterification 1, the top of reaction kettle of the esterification 1 Center is equipped with stirring port 1c, and the side of stirring port 1c is equipped with slurry import 1a and gaseous phase outlet 1b, in the bottom of reaction kettle of the esterification 1 The heart is equipped with catalyst inlet 1e, and the side of catalyst inlet 1e is equipped with evacuation port 1m.The inner cavity of reaction kettle of the esterification 1 is by ring baffle 1g is separated into mistress and interior room, and the lower central of interior room is equipped with inner cylinder 1n, heating is distributed in the annulus of the periphery inner cylinder 1n It includes from top to bottom that tubulation 1h, slurry import 1a, which are plugged with and protrude into slurry the inside extending tube 1f, slurry inside extending tube 1f of reaction kettle inner cavity, Vertical section, segmental arc and the tilting section being linked together, the lower port of tilting section are located at right above the inner cavity of inner cylinder 1n and apart from anti- Kettle highest 100~150mm of liquid level is answered, the bending radius of slurry inside extending tube segmental arc is six to ten times of slurry inside extending tube internal diameter.
The bending radius of segmental arc is six to ten times of slurry inside extending tube internal diameter, it is ensured that the flowing of fresh slurry is smooth, Sluggish or buildup will not occur at turning;Fresh slurry is directed to right above the inner cavity of inner cylinder 1n through slurry inside extending tube 1f, can Guarantee that whole raw materials each fall within the inner cavity of inner cylinder 1n, be stirred until homogeneous on one side in inner cylinder 1n with material in kettle, on one side to dirty It is dynamic, heating tubulation 1h is entered after the outflow of the lower edge of inner cylinder 1n, is flowed up while heating reaction, heating tubulation 1h heating The heat power of formation maintains Natural Circulation of the material inside and outside inner cylinder 1n.The utility model, which does not have fresh slurry and falls in, to be added Carbonized on the shell of hot tubulation 1h because of overheat, the lower port of slurry inside extending tube 1f only apart from reaction kettle highest liquid level 100~ 150mm not only can avoid raw material and be pumped because of negative pressure, but also charging blockage influences production when high liquid level being avoided to produce.
Reaction kettle of the esterification 1 is up big and down small structure, and the lower end of ring baffle 1g is welded on the kettle wall of heating tubulation 1h upper limb On, the top of ring baffle 1g is equipped with discharging seam 1g1, and kettle wall corresponding with the root ring baffle 1g is equipped with discharge port 1d, out Radial partition 1g2 is equipped between material seam 1g1 and discharge port 1d.The PBT of end of reaction stitches 1g1 from the discharging on the top ring baffle 1g It overflows, the radially barrier of partition 1g2, PBT flows after a week along annular groove, flows out from discharge port 1d.
Each heating tubulation 1h is vertically extending and penetrates through, the kettle wall lower part where heating tubulation 1h be connected with tubulation heating agent into Mouth 1j, the kettle wall top where heating tubulation 1h are connected with tubulation heating agent outlet 1k.Material along it is each heating tubulation 1h tube side to Upper flowing, heating agent such as conduction oil walk the shell side outside tubulation, and the heating of heating agent makes material be formed in the tube the power flowed up.
Barrel pump is built-in in catalyst bucket 6, the outlet of barrel pump passes through the feed inlet phase of barrel pump efferent duct G1 and catalyst tank 2 Even, the air inlet at 2 top of catalyst tank is connected with the outlet of nitrogen tube G2, and catalyst inlet 1e is equipped with catalyst rising pouring valve The discharge port 1d of V2, catalyst tank 2 are connected with the entrance of catalyst dosing pump 3, the outlet and catalyst mistake of catalyst dosing pump 3 The entrance of filter 4 is connected, and the outlet of catalyst filter 4 is connected with the material inlet of catalyst heater 5, catalyst heater 5 material outlet is connected by catalyst rising pouring pipe G4 with the entrance of catalyst rising pouring valve V2.
Butyl titanate sheet is easy conveying as liquid, and using this characteristic, the butyl titanate in catalyst bucket 6 is by bucket It pumps out, is entered in catalyst tank 2 by barrel pump efferent duct G1 and stored, the gas-phase space of catalyst tank 2 is filled with from nitrogen The nitrogen of pipe G2 protects catalyst, and the catalyst in catalyst tank 2 is directly extracted out and measured by catalyst dosing pump 3, It does not need to be prepared with BDO, while catalyst meets high-temperature evaporation suddenly in order to prevent, the catalyst that catalyst dosing pump 3 is sent out is through urging After agent filter 4 filters, it is preheating in 120 ~ 170 DEG C of feeding reaction kettle of the esterification 1 by catalyst heater 5.It is anti-due to being esterified A large amount of water should can be generated in reaction kettle of the esterification 1, the density of water is less than the density of PBT;Fresh catalyst passes through catalyst bottom It infuses pipe G4 and catalyst rising pouring valve V2 to inject from the bottom of reaction kettle of the esterification 1, can be contacted to avoid catalyst with water.
The Heating medium of catalyst heater 5 is equipped with steam control valve V3, the entrance and steam pipe of steam control valve V3 G3 is connected, and the material outlet of catalyst heater 5 is equipped with temperature sensor T1, and the aperture of steam control valve V3 is controlled by temperature The catalyst temperature that sensor T1 is measured;The heating agent outlet of catalyst heater 5 is connected with drip pipe G5.When temperature passes When the catalyst temperature of the outlet of catalyst heater 5 measured by sensor T1 is higher than setting upper limit value, then steam control valve V3 is opened Degree becomes smaller;When the catalyst temperature that the catalyst heater 5 measured by the temperature sensor T1 exports is lower than preset lower limit, then steam The aperture of steam control valve V3 increases, and can automatically keep the stabilization of catalyst temperature.
Catalyst bucket 6 is placed on transport trolley 7, and the outlet of barrel pump is connected by connecting hose with barrel pump efferent duct G1, is catalyzed The feed inlet of agent tank 2 is equipped with catalyst tank inlet valve V1, and the entrance of catalyst tank inlet valve V1 is connected with barrel pump efferent duct G1. Transport trolley 7 carries the inlet that catalyst bucket 6 reaches barrel pump efferent duct G1, after connecting using connecting hose, opens catalyst tank Inlet valve V1 can start barrel pump, to 2 injecting catalyst of catalyst tank.
The foregoing is merely the preferable possible embodiments of the utility model, patent that is non-therefore limiting to the utility model Protection scope.In addition to the implementation, the utility model can also have other embodiments, all to use equivalent replacement or equivalent change The technical solution to be formed is changed, is all fallen in the protection scope of the requires of the utility model.Technology of the utility model without description is special Sign can realize that details are not described herein by or using the prior art.

Claims (6)

1. the top center of a kind of PBT esterification device, including reaction kettle of the esterification, the reaction kettle of the esterification is equipped with stirring port, institute The side for stating stirring port is equipped with slurry import and gaseous phase outlet, and the inner cavity of the reaction kettle of the esterification is separated into mistress by ring baffle And interior room, the lower central of interior room are equipped with inner cylinder, heating tubulation are distributed in the annulus of the inner cylinder periphery, feature exists The slurry inside extending tube for protruding into reaction kettle inner cavity is plugged in: the slurry import, the slurry inside extending tube includes connecting from top to bottom Vertical section, segmental arc and the tilting section being integrated, the lower port of the tilting section be located at right above the inner cavity of the inner cylinder and away from From 100~150mm of reaction kettle highest liquid level, the bending radius of the slurry inside extending tube segmental arc is the six of slurry inside extending tube internal diameter To ten times.
2. PBT esterification device according to claim 1, it is characterised in that: the reaction kettle of the esterification is up big and down small knot Structure, the lower end of the ring baffle are welded on the kettle wall of the heating tubulation upper limb, and the top of the ring baffle is equipped with Material seam, kettle wall corresponding with ring baffle root are equipped with discharge port, are equipped between the discharging seam and the discharge port radial Partition.
3. PBT esterification device according to claim 1, it is characterised in that: each heating tubulation is vertically extending and penetrates through, Kettle wall lower part where heating tubulation is connected with tubulation Heating medium, and the kettle wall top where heating tubulation is connected with tubulation heating agent Outlet.
4. PBT esterification device according to claim 1 or 2 or 3, it is characterised in that: the bottom of the reaction kettle of the esterification Center is equipped with catalyst inlet, and the catalyst inlet is equipped with catalyst rising pouring valve;Barrel pump is built-in in catalyst bucket, it is described The outlet of barrel pump is connected by barrel pump efferent duct with the feed inlet of catalyst tank, air inlet and nitrogen at the top of the catalyst tank The outlet of pipe is connected, and the discharge port of the catalyst tank is connected with the entrance of catalyst dosing pump, the catalyst dosing pump Outlet is connected with the entrance of catalyst filter, the outlet and the material inlet phase of catalyst heater of the catalyst filter Even, the material outlet of the catalyst heater is connected by catalyst rising pouring pipe with the entrance of the catalyst rising pouring valve.
5. PBT esterification device according to claim 4, it is characterised in that: the Heating medium of the catalyst heater Steam control valve is installed, the entrance of the steam control valve is connected with steam pipe, the material outlet of the catalyst heater Temperature sensor is installed, the aperture of the steam control valve is controlled by the catalyst temperature that the temperature sensor measures;Institute The heating agent outlet for stating catalyst heater is connected with drip pipe.
6. PBT esterification device according to claim 4, it is characterised in that: the catalyst bucket is placed on transport trolley, The outlet of the barrel pump is connected by connecting hose with the barrel pump efferent duct, and the feed inlet of the catalyst tank is equipped with catalyst Tank inlet valve, the entrance of the catalyst tank inlet valve are connected with the barrel pump efferent duct.
CN201920053188.4U 2019-01-14 2019-01-14 A kind of PBT esterification device Active CN209530859U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114682196A (en) * 2020-12-31 2022-07-01 中国石油化工集团公司 Esterification reaction kettle and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114682196A (en) * 2020-12-31 2022-07-01 中国石油化工集团公司 Esterification reaction kettle and application thereof
CN114682196B (en) * 2020-12-31 2024-06-07 中国石油化工集团公司 Esterification reaction kettle and application thereof

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Address after: No. 301, Wangjiang Road, economic and Technological Development Zone, Yangzhou City, Jiangsu Province

Patentee after: Yangzhou Huitong Technology Co.,Ltd.

Address before: No. 301, Wangjiang Road, economic and Technological Development Zone, Yangzhou City, Jiangsu Province

Patentee before: YANGZHOU HUITONG CHEMICAL TECHNOLOGY Co.,Ltd.