CN105561905A - Esterification and polymerization two-kettle system - Google Patents

Esterification and polymerization two-kettle system Download PDF

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Publication number
CN105561905A
CN105561905A CN201610097833.3A CN201610097833A CN105561905A CN 105561905 A CN105561905 A CN 105561905A CN 201610097833 A CN201610097833 A CN 201610097833A CN 105561905 A CN105561905 A CN 105561905A
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esterification
precondensation
room
polymer reactor
under
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CN105561905B (en
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景辽宁
严旭明
陈文兴
刘荣俊
钟明
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Yangzhou Huitong Technology Co.,Ltd.
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Open Chemical Industry Technological Co Ltd Of Favor Of Yangzhou
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/14Production of inert gas mixtures; Use of inert gases in general
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polyesters Or Polycarbonates (AREA)

Abstract

The invention relates to an esterification and polymerization two-kettle system. A pre-polycondensation material outlet of an esterification and polymerization reactor is connected with a polymerization reactor feeding opening through a pre-polycondensation liquid level control valve or a pre-polycondensation melt conveying pump. The upper portion of an inner cavity of a polymerization reactor is provided with a liquid distribution disc, liquid distribution holes are internally provided with falling-film tubes, heat medium heating tubes are inserted into inner cavities of the falling-film tubes, the outer wall of the upper portion of a cylinder is provided with a polymerization reactor feeding inlet and a vacuumizing opening, the bottom of the polymerization reactor is provided with a discharging screw and a polymer outlet, the portion, corresponding to the polymerization reactor feeding inlet, of the inner wall of the cylinder is provided with an annular liquid distribution groove, and even annular gaps are reserved in the lower end of the liquid distribution groove; the inner wall of the lower portion of the cylinder is provided with a liquid collecting groove; the outer wall of the cylinder is provided with a middle melt outlet communicated with the liquid collecting groove, the middle melt outlet is connected with a middle melt inlet through a middle melt conveying pump, and the middle melt inlet is formed above the liquid distribution disc. The esterification and polymerization two-kettle system is compact in structure, small in occupied area and high in production efficiency.

Description

A kind of fat polymerization two still system
Technical field
The present invention relates to a kind of fat polymerization two still system, belong to polyester producing process field.
Background technology
In prior art, esterification during production of polyester and polycondensation reaction are generally carried out in separate reaction tower or reactor, if publication number is the Chinese invention patent of CN101618304B, disclose a kind of esterifier, be made up of polylith column plate, every block column plate is all installed a downspout and a riser, riser connects rotatable gas distributor, and gas distributor is made up of air entraining pipe, fan blades and nozzle.Every block column plate all retains the liquid of certain liquid level, has solid catalyst in liquid.Liquid phase is the component containing carboxylic acid, in the reactor downward by one block of esterification column plate current to next block column plate, with rise alcohol steam counter-flow react.
Publication number is the Chinese invention patent of CN2741645, disclose a kind of polycondensation reaction tower in polycondensation reaction device field, comprise the double Shell be made up of inner housing and shell body, it is chuck between inner housing and shell body, shell body is provided with the heating agent being communicated with chuck and enters, outlet, double Shell is provided with the steam outlet port being communicated with inner housing inner chamber, charging aperture and discharging opening, described double Shell is uprightly arranged, charging aperture is arranged at double Shell top and stretches in inner housing, discharging opening is arranged at the bottom of double Shell, some horizontally disposed tower trays are provided with between charging aperture and discharging opening, described tower tray comprises housing, some leakages material passage is provided with in housing.Esterification and polycondensation reaction are divided into two reactors and carry out traditionally, and structure is compact not, and floor space is large, and production efficiency is low.
Traditional polymer reactor comprises the cylindrical shell of vertical setting and closed at both ends, the top of polymer reactor inner chamber is provided with horizontal material distribution plate, material distribution plate is provided with material distribution hopper, the film supplying tube of closed at both ends is provided with and gap uniformity between the two in material distribution hopper, film supplying tube extends straight down and upper end is stretched out outside the top of polymer reactor, the inner chamber of film supplying tube is provided with heating medium for heating pipe, the external wall of upper portion of polymer reactor is provided with polymer reactor charging aperture and vacuum orifice, the conical lower portion of polymer reactor is provided with polymer discharge mouth, the periphery of polymer reactor is provided with heating jacket.
After PET melt enters polymer reactor inner chamber, drop on material distribution plate, flow out downwards from the material distribution hopper material distribution plate and the gap between film supplying tube, wall built-up falling liquid film is formed at the outer wall of film supplying tube, in film supplying tube thermal medium heating under, after melt completes polymerization, drop on bottom polymer reactor, then flow out from the polymer discharge mouth bottom polymer reactor.In course of reaction, pumped vacuum systems makes to keep vacuum state in polymer reactor by vacuum orifice.
After PET melt enters polymer reactor inner chamber, the Area comparison heated is little, and only carries out a polymerisation, and reaction speed is slow, and production efficiency is low; The Small molecular that reaction produces, easily in the carbonization of still wall, falls in the middle of material, and produce stain material, often need parking to wash still, unstable product quality, the cycle of operation is short.
Summary of the invention
The object of the invention is to, overcome problems of the prior art, provide a kind of fat polymerization two still system, compact conformation, production efficiency is high.
For solving above technical problem, a kind of fat polymerization two still system of the present invention, comprise esterification Prepolycondensating reactor and without stirring polymer reactor, described esterification Prepolycondensating reactor is provided with material inlet and precondensation discharging opening, described nothing stirs polymer reactor and is provided with polymer reactor charging aperture and polymer discharge mouth, described precondensation discharging opening is connected with precondensation discharge nozzle by precondensation fluid level control valve or precondensation melt Conveying pump, described precondensation discharge nozzle is connected with described polymer reactor charging aperture, the described cylindrical shell comprising vertical setting and closed at both ends without stirring polymer reactor, the top of cylinder lumen is provided with cloth liquid dish that is horizontal and that laterally cut off by cylindrical shell, described cloth liquid dish is provided with up big and down small liquid distributing hole, film supplying tube is provided with and both coaxial lines in described liquid distributing hole, described film supplying tube extends straight down, the inner chamber of described film supplying tube is plugged with polymer reactor heating medium for heating pipe, the external wall of upper portion of described cylindrical shell is provided with polymer reactor vacuum orifice and described polymer reactor charging aperture, the lower end of described cylindrical shell is provided with conical head, the lower end of described conical head is provided with discharging spiral, described polymer discharge mouth is positioned at the lower end of described discharging spiral, the periphery of described cylindrical shell is provided with polymer reactor chuck, the periphery of described conical head is provided with conical head chuck, described polymer reactor charging aperture is positioned at the below of described cloth liquid dish, the inwall of the described cylindrical shell position corresponding to described polymer reactor charging aperture is provided with the cloth liquid bath of ring-type, leaves uniform annular slot between the lower end of described cloth liquid bath and cylinder inboard wall, the lower inner wall of described cylindrical shell is provided with the collecting tank of ring-type, the upper end open of described collecting tank and lower end closed, the outer wall of described cylindrical shell is provided with the middle melt outlet communicated with the bottom of described collecting tank, described middle melt outlet is connected with the entrance of middle melt Conveying pump, described middle melt Conveying delivery side of pump is connected with middle melt inlet, and described middle melt inlet to be positioned on cylinder body outer wall and to be positioned at the top of described cloth liquid dish.
Relative to prior art, the present invention achieves following beneficial effect: when adopting precondensation fluid level control valve, precondensation melt enters polymer reactor charging aperture by potential difference; When adopting precondensation melt Conveying pump, carried to polymer reactor charging aperture by precondensation melt Conveying pump.Precondensation melt enters cloth liquid bath from polymer reactor charging aperture, with cloth liquid bath being circumferentially uniformly distributed at cylinder inboard wall, then flow out from the annular slot of cloth liquid bath lower end, cylinder inboard wall is formed uniform falling liquid film, in flow process, in chuck heating agent heating under, melt intensification is able to prepolymerization becomes melt in the middle of prepolymerization, then flow in the collecting tank of cylinder inboard wall bottom, then flow out from middle melt outlet, the middle melt inlet on polymer reactor top is pumped into again by middle melt Conveying, after entering polymer reactor inner chamber from middle melt inlet, drop on cloth liquid dish, flow out downwards from the liquid distributing hole cloth liquid dish and the gap between film supplying tube, wall built-up falling liquid film is again formed at the outer wall of film supplying tube, in film supplying tube thermal medium heating under, in the middle of prepolymerization, melt has been polymerized further, flow out from the polymer discharge mouth bottom polymer reactor.This polymer reactor adopts without stirring structure, power consumption and failure rate is low; Adopt ring-type cloth liquid bath cloth liquid at polymer reactor inner chamber, the falling liquid film of formation is even, and has carried out twice polymerization at polymer reactor inner chamber, improves reaction efficiency; In reaction and discharging process, bled by polymer reactor vacuum orifice, polymer reactor inner chamber remains at vacuum state, melt can not be caused to degrade, product with stable quality.
As improvement of the present invention, the top of described cloth liquid dish is provided with film supplying tube dividing plate, the top of described film supplying tube dividing plate is provided with polymer reactor heating medium for heating pipe dividing plate, cylindrical shell laterally cuts off by described film supplying tube dividing plate and described polymer reactor heating medium for heating pipe dividing plate respectively, and the top of described polymer reactor heating medium for heating pipe dividing plate is provided with polymer reactor upper cover; The upper port of described film supplying tube is connected on the pore of described film supplying tube dividing plate, and the upper port of described polymer reactor heating medium for heating pipe is connected on the pore of described polymer reactor heating medium for heating pipe dividing plate; Described polymer reactor upper cover is connected with film supplying tube Heating medium, the barrel wall between described film supplying tube dividing plate and polymer reactor heating medium for heating pipe dividing plate is connected with film supplying tube heating agent and exports.Thermal medium such as conduction oil enters the oil suction chamber between polymer reactor upper cover and polymer reactor heating medium for heating pipe dividing plate from film supplying tube Heating medium, then directly lower bottom polymer reactor heating medium for heating pipe along polymer reactor heating medium for heating pipe, the ring cavity between film supplying tube and polymer reactor heating medium for heating pipe is entered on outflow polymer reactor heating medium for heating pipe is backward, up along this ring cavity, enter from the upper port of film supplying tube and go out oil pocket between film supplying tube dividing plate and polymer reactor heating medium for heating pipe dividing plate, finally flow out from the outlet of film supplying tube heating agent.When material has just entered liquid distributing hole, temperature is lower, and flow downward along film supplying tube after forming falling liquid film, be constantly subject to the heating of heating agent in film supplying tube, temperature raises gradually, and when arriving bottom film supplying tube, the temperature of material reaches the highest.The highest heating agent of temperature first under bottom film supplying tube because the periphery of polymer reactor heating medium for heating pipe is the heating agent of return, temperature is higher, and the heating agent thermal loss descending along polymer reactor heating medium for heating pipe is very little; The up heating agent of return is owing to constantly carrying out heat release to material falling liquid film, and temperature declines gradually.Therefore the temperature of the outer material of film supplying tube increases progressively from top to bottom gradually, heat medium temperature in film supplying tube successively decreases from bottom to top gradually, the material that temperature is minimum and the lower heating agent of temperature carry out heat exchange, the material that temperature is the highest and the highest heating agent of temperature carry out heat exchange, heat exchange both sides remain the larger temperature difference, and heat exchange efficiency is high.
As a further improvement on the present invention, the barrel material that described cylinder inboard wall is provided with screw downward-extension distributes ring, the upper end that described barrel material distributes ring is positioned at below the outlet of described cloth liquid bath, the lower end that described barrel material distributes ring is positioned at above the upper port of described collecting tank, and described barrel material distribution ring is semi-circular cross-section and plane is connected on described cylinder inboard wall.Melt flows out from the annular slot of cloth liquid bath lower end, after flow downward formation falling liquid film along cylinder inboard wall, the barrel material crossing multiple tracks semi-circular cross-section is needed to distribute ring, blocked when crossing barrel material and distributing ring, make the falling liquid film thickness of the whole circumferencial direction of cylinder inboard wall and short transverse more even; Semi-circular cross-section smooth surface makes melt flows very evenly mild, there is not material dead angle again, avoids material stagnation to cause overheated.
As a further improvement on the present invention, the film supplying tube outer wall below described liquid distributing hole is evenly provided with at least one film supplying tube material and distributes ring, and the cross section that described film supplying tube material distributes ring is the little cydariform broad in the middle in two.Middle melt flows out downwards from the liquid distributing hole cloth liquid dish and the gap between film supplying tube, after the outer wall of film supplying tube forms wall built-up falling liquid film again, in the process of flowing downward, need the film supplying tube material crossing multiple tracks cydariform to distribute ring, blocked when crossing film supplying tube material and distributing ring, make the falling liquid film thickness of the whole circumferencial direction of film supplying tube outer wall and short transverse more even; The smooth surface arc-shaped transition that film supplying tube material distributes ring makes melt flows very evenly mild, there is not material dead angle again, avoids material stagnation to cause overheated.
As a further improvement on the present invention, described esterification Prepolycondensating reactor comprises closed vertical tower body, be separated in esterification that under room and precondensation room in described vertical tower body by arc-shaped partition, in described esterification room barrel outside be provided with esterification heating jacket, under described precondensation room barrel outside be provided with precondensation heating jacket; In described esterification, the top of room is provided with room gaseous phase outlet and described material inlet in esterification, and the bottom centre of described arc-shaped partition is provided with nitrogen inlet, and in described esterification, the sidewall of room is provided with esterification material outlet; Under described precondensation, the bottom of room is connected with esterification material preheater, preheater charging aperture is provided with bottom the low head of described esterification material preheater, described esterification material outlet is connected with described preheater charging aperture with carboxylate discharge nozzle by esterifying liquid level control valve, described carboxylate discharge nozzle is connected with auxiliary agent import, and the preheater discharging opening of described esterification material preheater upper end is connected with the bottom inlet of room under described precondensation; Under described precondensation, the inner chamber of room is provided with multilayer tower tray from bottom to top, and described precondensation discharging opening is positioned on the top barrel of room under described precondensation, and the top of described precondensation discharging opening is provided with room vacuum orifice under precondensation.Room esterification is entered from material inlet after PTA powder and ethylene glycol mixing making beating, nitrogen enters room esterification from the nitrogen inlet bottom arc-shaped partition, carrying out stirring to material makes it mix, in esterification room hot environment under, PTA powder and ethylene glycol generation esterification, in esterification, the operating pressure of room is 0.5 ~ 2bar(gauge pressure), the gaseous substance that esterification produces is discharged from room gaseous phase outlet esterification, esterification material is discharged from esterification material outlet, carboxylate discharge nozzle is entered by esterifying liquid level control valve, auxiliary agent adds in carboxylate discharge nozzle by auxiliary agent import, under the effect of potential difference and pressure reduction, esterification material and auxiliary agent enter preheater charging aperture, and in esterification material preheater, ethylene glycol gasification excessive in auxiliary agent produces bubble, and bubble from bottom to top moves to material with motive force, plays stirring action simultaneously, esterification material heated backward on enter room under precondensation, proceed partial esterification reaction, enter polycondensation process simultaneously, under precondensation room precondensation under room vacuum orifice be positioned at topmost, more higher toward upper strata vacuum, under precondensation, the vacuum at top, room is 1 ~ 10kpa(absolute pressure), material is progressively carrying out polymerisation through during tower tray layer by layer, material degree of polymerization in process from bottom to top is progressively increased, finally discharges from precondensation discharging opening.Esterification room and precondensation room are connected as a single entity by this reactor, compact conformation, and floor space is little, heat loss is few, can flow to room under precondensation, mechanical agitating device without the need to extra power material from room esterification, save energy consumption, reduced fault rate, improve production efficiency.
As a further improvement on the present invention, in described esterification, the bottom centre of room is provided with and is horizontally disposed with and the cyclone agitator disk be centrosymmetric, described cyclone agitator disk is hollow cylinder plate, the bottom centre of described cyclone agitator disk is connected with described nitrogen inlet, the circumferential wall of described cyclone agitator disk is evenly distributed with multiple nitrogen jet mouth, the outside of each described nitrogen jet mouth is respectively equipped with the nitrogen water conservancy diversion arc that nitrogen is tangentially penetrated, and the root of each described nitrogen water conservancy diversion arc is connected in the circumferential wall of described cyclone agitator disk.Nitrogen enters the inner chamber of cyclone agitator disk from the bottom centre of cyclone agitator disk, spray from each nitrogen jet mouth, through the water conservancy diversion of nitrogen water conservancy diversion arc, nitrogen all penetrates along the tangential direction of nitrogen water conservancy diversion arc tip circle everywhere, in esterification, horizontal vortex is formed on the bottom of room, can stir material fully, also will move upward after nitrogen injection to material formation secondary agitation, ensure that material thoroughly mixes.
As a further improvement on the present invention, in described esterification, the inner wall lower of room is provided with circumferentially and the external flow guiding cylinder of upper end open, described external flow guiding cylinder and esterification form esterification discharging annular groove between chamber interior walls, described external flow guiding cylinder is provided with external flow guiding cylinder material outlet and communicates with described esterification discharging annular groove, and described esterification material outlet communicates with the bottom of described esterification discharging annular groove; The inner chamber of described external flow guiding cylinder is provided with the inner draft tube of coaxial line with it, and the annular section between described inner draft tube and described external flow guiding cylinder is positioned at above the excircle of described cyclone agitator disk, and the upper port of described inner draft tube is lower than the upper port of external flow guiding cylinder; In described esterification, the inner chamber of room is provided with and expects to manage along the axis center extended downward in the middle part of inner draft tube, and the upper end of described center material pipe is connected with described material inlet; Between described external flow guiding cylinder and inner draft tube, annulus is provided with and organizes esterification heat(ing) coil more, often organizes heating medium for heating coil pipe and is respectively equipped with esterification heat(ing) coil Heating medium and the outlet of esterification heat(ing) coil heating agent.The nitrogen of cyclone agitator disk injection makes the material in esterification bottom room form strong circulation, and under the thermal convection current double action of nitrogen and heat(ing) coil, material moves upward along the annulus between inner draft tube and external flow guiding cylinder; The material of inner draft tube inside flows downward, and forms the state of inside and outside stream circulation, and namely new material is involved in stream circulation and is stirred after flowing out downwards from the lower port of center material pipe; At high temperature PTA powder and ethylene glycol generation esterification, along with new material constantly enters, the material reacted enters esterification discharging annular groove from the external flow guiding cylinder material outlet of external flow guiding cylinder, in esterification heating jacket heating agent heating current downflow process in continue reaction thoroughly, finally discharge from the esterification material outlet bottom esterification discharging annular groove.PTA powder and ethylene glycol between external flow guiding cylinder and inner draft tube in annulus while stir, esterified still heat(ing) coil heating, and can need according to technique the group number determining the esterifying kettle heat(ing) coil dropping into heating.
As a further improvement on the present invention, described external flow guiding cylinder material outlet along the short transverse of described external flow guiding cylinder vertically to downward-extension, the inner chamber of described esterification discharging annular groove is provided with the radial diaphragm in room, and described external flow guiding cylinder material outlet and described esterification material outlet lay respectively at the both sides of the radial diaphragm in described upper room; The top of top tray is provided with discharging annular groove in room under precondensation, under described precondensation, the bottom of room discharging annular groove is connected on the barrel of room under described precondensation, under described precondensation, room discharging annular groove is provided with room flash mouth under the precondensation vertically extended, described precondensation discharging opening communicates with the bottom of room discharging annular groove under described precondensation, under described precondensation, the inner chamber of room discharging annular groove is provided with the radial diaphragm in room under precondensation, and under described precondensation, room flash mouth and described precondensation discharging opening lay respectively at the both sides of room radial direction diaphragm under described precondensation.Esterification material outlet and external flow guiding cylinder material outlet separate by the radial diaphragm in upper room, can prevent the material in esterification discharging annular groove from short stream occurring, material is made to have maximum stroke in esterification discharging annular groove, material is the form of laminar flow after entering esterification discharging annular groove, along tower body inner wall surrounding one week, material continues the heating of esterified heating jacket in advance process, finally goes out from esterification material outlet flow, this structure to prolong heat time of material in esterification discharging annular groove.Under precondensation, flash mouth in room under precondensation and precondensation discharging opening separate by the radial diaphragm in room, can prevent the material under precondensation in room discharging annular groove from short stream occurring, material is made to have maximum stroke in room discharging annular groove under precondensation, material enters the form in laminar flow after room discharging annular groove under precondensation, along tower body inner wall surrounding one week, material continues to be heated by precondensation heating jacket in advance process, finally to flow out from precondensation discharging opening, this structure to prolong heat time of material under precondensation in room discharging annular groove.
As a further improvement on the present invention, the described tower tray of each layer is evenly distributed with respectively the material tedge of multiple through tower tray, the top of each described material tedge is coated with the material deflector cup of coaxial line with it respectively, each described material deflector cup is fornix shape and lower port is connected on described tower tray, and the lower circumference of each described material deflector cup is evenly provided with deflector cup discharging opening.Material is advanced into the inner chamber of material deflector cup from material tedge, and then baffling flows out from the deflector cup discharging opening material deflector cup lower circumference downwards.Due to the swabbing action of room vacuum orifice and the polycondensation process of material under top, room precondensation under precondensation, air cavity is formed at the top of every one deck material deflector cup, vacuum in most last layer material deflector cup air cavity is the highest, vacuum more down in material deflector cup air cavity is progressively successively decreased, material is from bottom to top successively by progressively carrying out polymerisation in the process of each layer tower tray and material deflector cup, and material degree of polymerization in process from bottom to top progressively increases.
As a further improvement on the present invention, under described precondensation, the top of room discharging annular groove is provided with foam trapping dish, the below of room vacuum orifice on the cross section that described foam trapping dish is horizontally set on room under described precondensation and under being positioned at described precondensation; The low head inner chamber of described esterification material preheater is respectively equipped with horizontally disposed material distribution plate, and described material distribution plate is evenly distributed with multiple material dispensing orifice.Can produce a large amount of bubble in polymerization process, foam trapping dish can stop the bubble of room under precondensation to enter under the precondensation of top room vacuum meter interface under room vacuum orifice and precondensation.Esterification material and auxiliary agent, after numerous material dispensing orifices of material distribution plate, more uniformly can enter each heat exchanging pipe of top.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation, and accompanying drawing only provides reference and explanation use, is not used to limit the present invention.
Fig. 1 is the schematic diagram of the first embodiment of fat polymerization two still system of the present invention.
Fig. 2 is the schematic diagram of fat polymerization two still system the second embodiment of the present invention.
Fig. 3 is the structural representation of polymer reactor of the present invention.
Fig. 4 is the enlarged drawing at A position in Fig. 3.
Fig. 5 is the structural representation of esterification Prepolycondensating reactor in Fig. 1.
Fig. 6 is the flow direction of material figure of esterification discharging annular groove in Fig. 5.
Fig. 7 is the sectional view of cyclone agitator disk in Fig. 5.
Fig. 8 is the structural representation of material distribution plate in Fig. 5.
Fig. 9 is the enlarged drawing at B position in Fig. 5.
Figure 10 is the flow direction of material figure of discharging annular groove in room under precondensation in Fig. 5.
In figure: 1. room in esterification; 1a. material inlet; Room gaseous phase outlet in 1b. esterification; 1c. nitrogen inlet; 1d. external flow guiding cylinder; 1d1. external flow guiding cylinder material outlet; 1e. esterification discharging annular groove; The radial diaphragm in the upper room of 1e1.; 1f. esterification material outlet; 1g. inner draft tube; 1h. cyclone agitator disk; 1h1. nitrogen jet mouth; 1h2. nitrogen water conservancy diversion arc; Room interface of the level gauge in 1j. esterification; Chamber pressure table interface in 1k. esterification; Room Heating medium in 1m. esterification; Heating agent outlet in room in 1n. esterification; 1p. esterification heat(ing) coil.
2. room under precondensation; 2a. tower tray; 2a1. material tedge; 2a2. material deflector cup; 2a3. deflector cup discharging opening; Discharging annular groove in room under 2b. precondensation; Flash mouth in room under 2b1. precondensation; The radial diaphragm in room under 2b2. precondensation; 2c. precondensation discharging opening; 2d. foam trapping dish; Room vacuum orifice under 2e. precondensation; Room interface of the level gauge under 2f. precondensation; Vacuum meter interface in room under 2g. precondensation; Room Heating medium under 2h. precondensation; Heating agent outlet in room under 2j. precondensation.
3. esterification material preheater; 3a. preheater charging aperture; 3b. preheater discharging opening; 3c. preheater Heating medium; 3d. preheater heating agent exports; 3e. material distribution plate; 3e1. material dispensing orifice.
B1. precondensation melt Conveying pump; G1. carboxylate discharge nozzle; G1a. auxiliary agent import; G2. precondensation discharge nozzle; V1. esterifying liquid level control valve; V2. precondensation fluid level control valve.
4. without stirring polymer reactor; 401a. polymer reactor charging aperture; 401b. polymer reactor vacuum orifice; Melt inlet in the middle of 401c.; Melt outlet in the middle of 401d.; 401e. polymer reactor heating medium for heating pipe dividing plate; 401f. film supplying tube dividing plate; 402. cloth liquid dishes; 402a. liquid distributing hole; 403. film supplying tube; 403a. film supplying tube material distributes ring; 404. cloth liquid baths; 405. collecting tank; 406. middle melt Conveying pumps; 407. polymer reactor chucks; 407a. polymer reactor chuck Heating medium; 407b. polymer reactor chuck heating agent exports; 408a. film supplying tube Heating medium; 408b. film supplying tube heating agent exports; 409a. conical head chuck Heating medium; 409b. conical head chuck heating agent exports; 410. discharging spirals; 410a. polymer discharge mouth; 411. polymer reactor heating medium for heating pipes; 412. barrel materials distribute ring; 413. collecting tank interface of the level gauge; 414. conical head interface of the level gauge.
Detailed description of the invention
Shown in Fig. 1, fat polymerization two still system of the present invention comprise esterification Prepolycondensating reactor and without stirring polymer reactor 4, esterification Prepolycondensating reactor is provided with material inlet 1a and precondensation discharging opening 2c, polymer reactor charging aperture 401a and polymer discharge mouth 410a is provided with without stirring polymer reactor 4, precondensation discharging opening 2c is connected with precondensation discharge nozzle G2 by precondensation fluid level control valve V2, and precondensation discharge nozzle G2 is connected with polymer reactor charging aperture 401a.
Shown in Fig. 2, fat polymerization two still system of the present invention comprise esterification Prepolycondensating reactor and without stirring polymer reactor 4, esterification Prepolycondensating reactor is provided with material inlet 1a and precondensation discharging opening 2c, polymer reactor charging aperture 401a and polymer discharge mouth 410a is provided with without stirring polymer reactor 4, precondensation discharging opening 2c is connected with precondensation discharge nozzle G2 by precondensation melt Conveying pump B1, and precondensation discharge nozzle G2 is connected with polymer reactor charging aperture 401a.
As shown in Figure 3 and Figure 4, the cylindrical shell of vertical setting and closed at both ends is comprised without stirring polymer reactor 4, the top of cylinder lumen is provided with cloth liquid dish 402 that is horizontal and that laterally cut off by cylindrical shell, and cloth liquid dish 402 is provided with liquid distributing hole 402a, is provided with film supplying tube 403 and both coaxial lines in liquid distributing hole 402a.Liquid distributing hole 402a is up big and down small infundibulate, is convenient to enough materials and flows in liquid distributing hole 402a, the thickness of the small end of liquid distributing hole 402a and the clearance control falling liquid film of film supplying tube 403.Film supplying tube 403 extends straight down, the inner chamber of film supplying tube 403 is plugged with polymer reactor heating medium for heating pipe 411, polymer reactor charging aperture 401a and polymer reactor vacuum orifice 401b is provided with without the cylindrical shell external wall of upper portion stirring polymer reactor 4, conical head is provided with without the lower end of stirring polymer reactor 4, the lower end of conical head is provided with discharging spiral 410, and the lower end of discharging spiral 410 is provided with polymer discharge mouth 410a.
Be provided with polymer reactor chuck 407 without the cylindrical shell periphery of stirring polymer reactor 4, the bottom of polymer reactor chuck 407 is provided with polymer reactor chuck Heating medium 407a, and the top of polymer reactor chuck 407 is provided with polymer reactor chuck heating agent outlet 407b.Heating agent enters in polymer reactor chuck 407 from polymer reactor chuck Heating medium 407a, then flows out from polymer reactor chuck heating agent outlet 407b.
The periphery of conical head is provided with conical head chuck, and the bottom of conical head chuck is provided with conical head chuck Heating medium 409a, and the top of conical head chuck is provided with conical head chuck heating agent outlet 409b.Heating agent enters in conical head chuck from conical head chuck Heating medium 409a, then flows out from conical head chuck heating agent outlet 409b.
Polymer reactor charging aperture 401a is positioned at the below of cloth liquid dish 402, be provided with the cloth liquid bath 404 of ring-type without the position that the cylinder inboard wall stirring polymer reactor 4 is corresponding to polymer reactor charging aperture 401a, between the lower end of cloth liquid bath 404 and cylinder inboard wall, leave uniform annular slot; Without the collecting tank 405 stirring the lower inner wall of polymer reactor 4 and be provided with ring-type, the upper end open of collecting tank 405 and lower end closed; The middle melt outlet 401d communicated with the bottom of collecting tank 405 is provided with without the outer wall stirring polymer reactor 4, middle melt outlet 401d is connected with the entrance of middle melt Conveying pump 406, the outlet of middle melt Conveying pump 406 is connected with middle melt inlet 401c, and middle melt inlet 401c to be positioned on cylinder body outer wall and to be positioned at the top of cloth liquid dish 402.
Middle melt outlet 401d and middle melt inlet 401c circumferentially evenly can be provided with one group, more than two groups or three groups nothing stirring polymer reactor 4.
Cloth liquid dish 402 can be provided with multiple liquid distributing hole 402a, and the center of each liquid distributing hole 402a is respectively equipped with film supplying tube 403.Film supplying tube 403 at least arranges one group, and often group is equipped with polymer reactor heating medium for heating pipe 411.
The top of cloth liquid dish 402 is provided with film supplying tube dividing plate 401f, the top of film supplying tube dividing plate 401f is provided with polymer reactor heating medium for heating pipe dividing plate 401e, cylindrical shell laterally cuts off by polymer reactor heating medium for heating pipe dividing plate 401e and film supplying tube dividing plate 401f respectively, and the top of polymer reactor heating medium for heating pipe dividing plate 401e is provided with polymer reactor upper cover; The upper port of film supplying tube 403 is connected on the pore of film supplying tube dividing plate 401f, and the upper port of polymer reactor heating medium for heating pipe 411 is connected on the pore of polymer reactor heating medium for heating pipe dividing plate 401e; Polymer reactor upper cover is connected with film supplying tube Heating medium 408a, the barrel wall between film supplying tube dividing plate 401f and polymer reactor heating medium for heating pipe dividing plate 401e is connected with film supplying tube heating agent and exports 408b.
Polymer reactor vacuum orifice 401b is positioned at the below of cloth liquid dish 402, and in reaction and discharging process, bled by polymer reactor vacuum orifice 401b, polymer reactor inner chamber remains at vacuum state.
Position corresponding with the lower end of collecting tank 405 on polymer reactor is provided with collecting tank interface of the level gauge 413, and the lower end of conical head is provided with conical head interface of the level gauge 414, to control the liquid level of polymer reactor materials inside.
Melt enters cloth liquid bath 404 from polymer reactor charging aperture 401a, with cloth liquid bath 404 being circumferentially uniformly distributed at cylinder inboard wall, then flow out from the annular slot of cloth liquid bath 404 lower end, cylinder inboard wall is formed uniform falling liquid film, in flow process, in polymer reactor chuck heating agent heating under, melt intensification is able to prepolymerization becomes melt in the middle of prepolymerization, then flow in the collecting tank 405 of cylinder inboard wall bottom, then flow out from middle melt outlet 401d, the middle melt inlet 401c on polymer reactor top is sent into again by middle melt Conveying pump 406, after entering polymer reactor inner chamber from middle melt inlet 401c, drop on cloth liquid dish 402, flow out downwards from the liquid distributing hole 402a cloth liquid dish 402 and the gap between film supplying tube 403, wall built-up falling liquid film is again formed at the outer wall of film supplying tube 403, in film supplying tube 403 thermal medium heating again under, in the middle of prepolymerization, melt has been polymerized further, discharging spiral 410 is entered from the conical head bottom polymer reactor, discharge from the polymer discharge mouth 410a of discharging spiral 410 lower end again.The esterification yield of polymer discharge mouth 410a is greater than 99%, and the degree of polymerization is greater than 100.
Thermal medium such as conduction oil enters the oil suction chamber between polymer reactor upper cover and polymer reactor heating medium for heating pipe dividing plate 401e from film supplying tube Heating medium 408a, then directly lower bottom polymer reactor heating medium for heating pipe 411 along polymer reactor heating medium for heating pipe 411, the ring cavity between film supplying tube 403 and polymer reactor heating medium for heating pipe 411 is entered on outflow polymer reactor heating medium for heating pipe 411 is backward, up along this ring cavity, enter from the upper port of film supplying tube 403 and go out oil pocket between film supplying tube dividing plate 401f and polymer reactor heating medium for heating pipe dividing plate 401e, finally flow out from film supplying tube heating agent outlet 408b.
When material has just entered liquid distributing hole 402a, temperature is lower, flows downward, be constantly subject to the heating of heating agent in film supplying tube 403 after forming falling liquid film along film supplying tube 403, and temperature continues to raise, and when arriving bottom film supplying tube 403, the temperature of material reaches the highest.And the highest heating agent of temperature is first lower bottom film supplying tube 403, because the periphery of polymer reactor heating medium for heating pipe 411 is the heating agent of return, temperature is higher, and the heating agent thermal loss descending along polymer reactor heating medium for heating pipe 411 is very little; The up heating agent of return is owing to constantly carrying out heat release to material falling liquid film, and temperature declines gradually.Therefore the temperature of the outer material of film supplying tube increases progressively from top to bottom gradually, heat medium temperature in film supplying tube successively decreases from bottom to top gradually, the material that temperature is lower and the lower heating agent of temperature carry out heat exchange, the material that temperature is the highest and the highest heating agent of temperature carry out heat exchange, heat exchange both sides remain the larger temperature difference, and heat exchange efficiency is high.This polymer reactor adopts ring-type cloth liquid bath 404 cloth liquid at polymer reactor inner chamber, at film supplying tube 403 outer employing liquid distributing hole 402a cloth liquid, the falling liquid film of formation is all very even, and has carried out twice polymerization at polymer reactor inner chamber, increase heat exchange area, improve reaction efficiency.
The barrel material that cylinder inboard wall is provided with screw downward-extension distributes ring 412, the upper end that barrel material distributes ring 412 is positioned at below the outlet of cloth liquid bath 404, the lower end that barrel material distributes ring 412 is positioned at above the upper port of collecting tank 405, and barrel material distribution ring 412 is semi-circular cross-section and plane is connected on cylinder inboard wall.Melt flows out from the annular slot of cloth liquid bath 404 lower end, after flow downward formation falling liquid film along cylinder inboard wall, the barrel material crossing multiple tracks semi-circular cross-section is needed to distribute ring 412, blocked when crossing barrel material and distributing ring 412, make the falling liquid film thickness of the whole circumferencial direction of cylinder inboard wall and short transverse more even; Semi-circular cross-section smooth surface makes melt flows very evenly mild, there is not material dead angle again, avoids material stagnation to cause overheated.
Film supplying tube 403 outer wall below liquid distributing hole is evenly provided with at least one film supplying tube material and distributes ring 403a, and the cross section that film supplying tube material distributes ring 403a is the little cydariform broad in the middle in two.Middle melt flows out downwards from the liquid distributing hole cloth liquid dish 402 and the gap between film supplying tube 403, after the outer wall of film supplying tube 403 forms wall built-up falling liquid film again, in the process of flowing downward, need the film supplying tube material crossing multiple tracks cydariform to distribute ring 403a, blocked when crossing film supplying tube material and distributing ring 403a, make the falling liquid film thickness of the whole circumferencial direction of film supplying tube outer wall and short transverse more even; The smooth surface arc-shaped transition that film supplying tube material distributes ring 403a makes melt flows very evenly mild, there is not material dead angle again, avoids material stagnation to cause overheated.
As shown in Fig. 5 to Figure 10, esterification Prepolycondensating reactor comprises closed vertical tower body, be separated in esterification that under room 1 and precondensation room 2 in vertical tower body by arc-shaped partition, in esterification room 1 barrel outside be provided with esterification heating jacket, under precondensation room 2 barrel outside be provided with precondensation heating jacket; In esterification, the top of room 1 is provided with gaseous phase outlet 1b in room in material inlet 1a and esterification, and the bottom centre of arc-shaped partition is provided with nitrogen inlet 1c, and in esterification, the sidewall of room 1 is provided with esterification material outlet 1f, and in esterification, the top of room 1 is provided with chamber pressure table interface 1k in esterification.
Under precondensation, the bottom of room 2 is connected with esterification material preheater 3, preheater charging aperture 3a is provided with bottom the low head of esterification material preheater 3, esterification material outlet 1f is connected with carboxylate discharge nozzle G1 by esterifying liquid level control valve V1 or precondensation melt Conveying pump B1, carboxylate discharge nozzle G1 is connected with preheater charging aperture 3a, carboxylate discharge nozzle G1 is connected with auxiliary agent import G1a, the preheater discharging opening 3b of esterification material preheater 3 upper end is connected with the bottom inlet of room under precondensation 2.
Under precondensation, the inner chamber of room 2 is provided with multilayer tower tray 2a from bottom to top, under precondensation, the top barrel of room 2 is provided with precondensation discharging opening 2c, precondensation discharging opening 2c is connected with precondensation discharge nozzle G2 by precondensation fluid level control valve V2 or precondensation melt Conveying pump B1, and the top of precondensation discharging opening 2c to be provided with under precondensation room vacuum meter interface 2g under room vacuum orifice 2e and precondensation.
Room 1 esterification is entered from material inlet 1a after PTA powder and ethylene glycol mixing making beating, nitrogen enters room 1 esterification from the nitrogen inlet 1c bottom arc-shaped partition, carrying out stirring to material makes it mix, in esterification room 1 hot environment under, PTA powder and ethylene glycol generation esterification, in esterification, the operating pressure of room 1 is 0.5 ~ 2bar(gauge pressure), the gaseous substance that esterification produces is discharged from gaseous phase outlet 1b in room esterification, esterification material is discharged from esterification material outlet 1f, carboxylate discharge nozzle G1 is entered by esterifying liquid level control valve V1, auxiliary agent is added in carboxylate discharge nozzle G1 by auxiliary agent import G1a.Under the effect of potential difference and pressure reduction, esterification material and auxiliary agent enter preheater charging aperture 3a, and in esterification material preheater 3, ethylene glycol gasification excessive in auxiliary agent produces bubble, and bubble from bottom to top moves to material with motive force, plays stirring action simultaneously.Esterification material heated backward on enter room 2 under precondensation, proceed partial esterification reaction, enter polycondensation process simultaneously.Under precondensation room 2 precondensation under room vacuum orifice 2e be positioned at topmost, more higher toward upper strata vacuum, under precondensation, the vacuum at top, room is 1 ~ 10kpa(absolute pressure), material is progressively carrying out polymerisation through during tower tray layer by layer, material degree of polymerization in process from bottom to top is progressively increased, finally discharges from precondensation discharging opening 2c.
In esterification, the bottom centre of room 1 is provided with and is horizontally disposed with and the cyclone agitator disk 1h be centrosymmetric, cyclone agitator disk 1h is hollow cylinder plate, the bottom centre of cyclone agitator disk 1h is connected with nitrogen inlet 1c, the circumferential wall of cyclone agitator disk 1h is evenly distributed with multiple nitrogen jet mouth 1h1, the outside of each nitrogen jet mouth 1h1 is respectively equipped with the nitrogen water conservancy diversion arc 1h2 that nitrogen is tangentially penetrated, and the root of each nitrogen water conservancy diversion arc 1h2 is connected in the circumferential wall of cyclone agitator disk 1h.Nitrogen enters the inner chamber of cyclone agitator disk 1h from the bottom centre of cyclone agitator disk 1h, spray from each nitrogen jet mouth 1h1, through the water conservancy diversion of nitrogen water conservancy diversion arc 1h2, nitrogen all penetrates along the tangential direction of nitrogen water conservancy diversion arc tip circle everywhere, in esterification, horizontal vortex is formed on the bottom of room 1, can stir material fully, also will move upward after nitrogen injection to material formation secondary agitation, ensure that material thoroughly mixes.
In esterification, the inner wall lower of room 1 is provided with circumferentially and the external flow guiding cylinder 1d of upper end open, external flow guiding cylinder 1d and esterification form esterification discharging annular groove 1e between the inwall of room 1, external flow guiding cylinder 1d is provided with external flow guiding cylinder material outlet 1d1 and communicates with esterification discharging annular groove 1e, and esterification material outlet 1f communicates with the bottom of esterification discharging annular groove 1e; The inner chamber of external flow guiding cylinder 1d is provided with the inner draft tube 1g of coaxial line with it, and the annular section between inner draft tube 1g and external flow guiding cylinder 1d is positioned at above the excircle of cyclone agitator disk 1h, and the upper port of inner draft tube 1g is lower than the upper port of external flow guiding cylinder 1d; In esterification, the inner chamber of room 1 is provided with and expects to manage along the axis center extended downward in the middle part of inner draft tube 1g, and the upper end of center material pipe is connected with material inlet 1a.
The nitrogen that cyclone agitator disk 1h penetrates makes the material in esterification bottom room form strong circulation, and under the thermal convection current double action of nitrogen and heat(ing) coil, material moves upward along the annulus between inner draft tube 1g and external flow guiding cylinder 1d; The material of inner draft tube 1g inside flows downward, and forms the state of inside and outside stream circulation, and namely new material is involved in stream circulation and is stirred after flowing out downwards from the lower port of center material pipe; At high temperature PTA powder and ethylene glycol generation esterification, along with new material constantly enters, the material reacted enters esterification discharging annular groove 1e from the external flow guiding cylinder material outlet 1d1 of external flow guiding cylinder 1d, in esterification heating jacket heating agent heating current downflow process in continue reaction thoroughly, finally discharge from the esterification material outlet 1f bottom esterification discharging annular groove 1e.
Between external flow guiding cylinder 1d and inner draft tube 1g, annulus is provided with and organizes esterification heat(ing) coil 1p more, often organizes heating medium for heating coil pipe and is respectively equipped with esterification heat(ing) coil Heating medium and the outlet of esterification heat(ing) coil heating agent.PTA powder and ethylene glycol between external flow guiding cylinder 1d and inner draft tube 1g in annulus while stir, esterified still heat(ing) coil heating, and can need according to technique the group number determining the esterifying kettle heat(ing) coil dropping into heating.
External flow guiding cylinder material outlet 1d1 along the short transverse of external flow guiding cylinder 1d vertically to downward-extension, the inner chamber of esterification discharging annular groove 1e is provided with the both sides that room radial diaphragm 1e1, external flow guiding cylinder material outlet 1d1 and esterification material outlet 1f lay respectively at the radial diaphragm 1e1 in room; The top of top tray is provided with room discharging annular groove 2b under precondensation, under precondensation, the bottom of room discharging annular groove 2b is connected on the barrel of room 2 under precondensation, under precondensation, room discharging annular groove 2b is provided with room flash mouth 2b1 under the precondensation vertically extended, precondensation discharging opening 2c communicates with the bottom of room discharging annular groove 2b under precondensation, under precondensation, the inner chamber of room discharging annular groove 2b is provided with the radial diaphragm 2b2 in room under precondensation, and under precondensation, room flash mouth 2b1 and precondensation discharging opening 2c lays respectively at the both sides of room radial direction diaphragm 2b2 under precondensation.
Esterification material outlet 1f and external flow guiding cylinder material outlet 1d1 separates by the radial diaphragm 1e1 in upper room, can prevent the material in esterification discharging annular groove 1e from short stream occurring, material is made to have maximum stroke in esterification discharging annular groove 1e, material is the form of laminar flow after entering esterification discharging annular groove 1e, along tower body inner wall surrounding one week, material continues the heating of esterified heating jacket in advance process, finally to flow out from esterification material outlet 1f, this structure to prolong heat time of material in esterification discharging annular groove 1e.Under precondensation, flash mouth 2b1 in room under precondensation and precondensation discharging opening 2c separates by the radial diaphragm 2b2 in room, can prevent the material under precondensation in room discharging annular groove 2b from short stream occurring, material is made to have maximum stroke in room discharging annular groove 2b under precondensation, material enters the form in laminar flow after room discharging annular groove 2b under precondensation, along tower body inner wall surrounding one week, material continues to be heated by precondensation heating jacket in advance process, finally to flow out from precondensation discharging opening 2c, this structure to prolong heat time of material under precondensation in room discharging annular groove 2b.
Under precondensation, the top of room discharging annular groove 2b is provided with foam trapping dish 2d, the below of room vacuum orifice 2e on the cross section that foam trapping dish 2d is horizontally set on room 2 under precondensation and under being positioned at precondensation.Can produce a large amount of bubble in polymerization process, foam trapping dish 2d can stop the bubble of room 2 under precondensation to enter under the precondensation of top room vacuum meter interface 2g under room vacuum orifice 2e and precondensation.
Each layer tower tray 2a is evenly distributed with respectively the material tedge 2a1 of multiple through tower tray, the top of each material tedge 2a1 is coated with the material deflector cup 2a2 of coaxial line with it respectively, each material deflector cup 2a2 is fornix shape and lower port is connected on tower tray 2a, and the lower circumference of each material deflector cup 2a2 is evenly provided with deflector cup discharging opening 2a3.Material is advanced into the inner chamber of material deflector cup 2a2 from material tedge 2a1, and then baffling flows out from the deflector cup discharging opening 2a3 material deflector cup 2a2 lower circumference downwards.Due to the swabbing action of room vacuum orifice 2e under top, room precondensation under precondensation and the polycondensation process of material, air cavity is formed at the top of every one deck material deflector cup 2a2, vacuum in most last layer material deflector cup air cavity is the highest, vacuum more down in material deflector cup air cavity is progressively successively decreased, material is from bottom to top successively by progressively carrying out polymerisation in the process of each layer tower tray and material deflector cup 2a2, and material degree of polymerization in process from bottom to top progressively increases.
The low head inner chamber of esterification material preheater 3 is respectively equipped with horizontally disposed material distribution plate 3e, material distribution plate 3e is evenly distributed with multiple material dispensing orifice 3e1.Esterification material and auxiliary agent, after numerous material dispensing orifice 3e1 of material distribution plate 3e, more uniformly can enter each heat exchanging pipe of top.
In esterification, the barrel of room 1 is provided with interface of the level gauge 1j in room in esterification and communicates with the bottom of esterification discharging annular groove 1e, and the aperture of esterifying liquid level control valve V1 is controlled by the liquid level of esterification discharging annular groove 1e; Under under precondensation, the barrel of room 2 is provided with precondensation, room interface of the level gauge 2f communicates with the bottom of room discharging annular groove 2b under precondensation, the liquid level of the aperture of precondensation fluid level control valve V2 or flow rates controlled room discharging annular groove 2b under precondensation of precondensation melt Conveying pump B1.
The bottom of esterification heating jacket is provided with Heating medium 1m in room in esterification, and the top of esterification heating jacket is provided with room heating agent outlet 1n in esterification; The bottom of precondensation heating jacket is provided with room Heating medium 2h under precondensation, and the top of precondensation heating jacket is provided with heating agent outlet 2j in room under precondensation; The shell side bottom of esterification material preheater 3 is provided with preheater Heating medium 3c, and the shell side top of esterification material preheater 3 is provided with preheater heating agent outlet 3d.
The job step of esterification Prepolycondensating reactor of the present invention is as follows successively: (1) PTA powder and ethylene glycol mixing making beating Hou Jing center material pipe enter the inner draft tube 1g of room 1 in esterification, nitrogen sprays from each nitrogen jet mouth 1h1 of cyclone agitator disk 1h, horizontal vortex is formed through the bottom of water conservancy diversion room 1 in esterification of nitrogen water conservancy diversion arc 1h2, nitrogen moves upward to material formation secondary agitation, material moves upward along the annulus between inner draft tube 1g and external flow guiding cylinder 1d under the thermal convection current double action of nitrogen and heat(ing) coil, the material of inner draft tube 1g inside flows downward, form inside and outside stream circulation.
(2) at high temperature there is esterification in PTA powder and ethylene glycol room 1 in esterification, and in esterification, the gauge pressure of room 1 is 0.5 ~ 2bar, and the gaseous substance that esterification produces is discharged from gaseous phase outlet 1b in room esterification; Along with new material constantly enters, the material reacted enters esterification discharging annular groove 1e from external flow guiding cylinder material outlet 1d1, flow one week in esterification discharging annular groove 1e and continue to be made reaction thorough by heating, finally discharge from esterification material outlet 1f, carboxylate discharge nozzle G1 is entered by esterifying liquid level control valve V1, the aperture of esterifying liquid level control valve V1 is controlled by the liquid level of esterification discharging annular groove 1e, and auxiliary agent is added to carboxylate discharge nozzle G1 from auxiliary agent import G1a.
(3), under the effect of potential difference and pressure reduction, esterification material and auxiliary agent enter preheater and through material distribution plate 3e, ethylene glycol gasification excessive in auxiliary agent produces bubble, and bubble moves upward and promotes material and stir; Esterification material heated backward on enter room 2 under precondensation.
(4) under precondensation, in room 2, material upwards proceeds partial esterification reaction through each floor tower tray successively, and enters polycondensation process; When through tower tray 2a, material is advanced into the inner chamber of material deflector cup 2a2 from material tedge 2a1, and then baffling flows out from the deflector cup discharging opening 2a3 material deflector cup lower circumference downwards, forms air cavity at the top of material deflector cup 2a2; Under precondensation, the absolute pressure at top, room is 1 ~ 10kpa, vacuum in most last layer material deflector cup air cavity is the highest, more progressively successively decrease, material degree of polymerization in process from bottom to top progressively increases, enter room discharging annular groove 2b under precondensation, flow one week in room discharging annular groove 2b under precondensation and continue to be heated, finally discharging from precondensation discharging opening 2c, enter precondensation discharge nozzle G2 by precondensation fluid level control valve V2 or precondensation melt Conveying pump B1.The material esterification yield of precondensation discharging opening 2c is greater than 96%, and the degree of polymerization is greater than 15.
The foregoing is only the better possible embodiments of the present invention, non-ly therefore limit to scope of patent protection of the present invention.In addition to the implementation, the present invention can also have other embodiments, and such as heating agent can be conduction oil, also can be other heat carrier etc.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop in the protection domain of application claims.The present invention can pass through without the technical characteristic described or adopt existing techniques in realizing, does not repeat them here.

Claims (10)

1. a fat polymerization two still system, comprise esterification Prepolycondensating reactor and without stirring polymer reactor, described esterification Prepolycondensating reactor is provided with material inlet and precondensation discharging opening, described nothing stirs polymer reactor and is provided with polymer reactor charging aperture and polymer discharge mouth, described precondensation discharging opening is connected with precondensation discharge nozzle by precondensation fluid level control valve or precondensation melt Conveying pump, described precondensation discharge nozzle is connected with described polymer reactor charging aperture, it is characterized in that: the described cylindrical shell comprising vertical setting and closed at both ends without stirring polymer reactor, the top of cylinder lumen is provided with cloth liquid dish that is horizontal and that laterally cut off by cylindrical shell, described cloth liquid dish is provided with up big and down small liquid distributing hole, film supplying tube is provided with and both coaxial lines in described liquid distributing hole, described film supplying tube extends straight down, the inner chamber of described film supplying tube is plugged with polymer reactor heating medium for heating pipe, the external wall of upper portion of described cylindrical shell is provided with polymer reactor vacuum orifice and described polymer reactor charging aperture, the lower end of described cylindrical shell is provided with conical head, the lower end of described conical head is provided with discharging spiral, described polymer discharge mouth is positioned at the lower end of described discharging spiral, the periphery of described cylindrical shell is provided with polymer reactor chuck, the periphery of described conical head is provided with conical head chuck, described polymer reactor charging aperture is positioned at the below of described cloth liquid dish, the inwall of the described cylindrical shell position corresponding to described polymer reactor charging aperture is provided with the cloth liquid bath of ring-type, leaves uniform annular slot between the lower end of described cloth liquid bath and cylinder inboard wall, the lower inner wall of described cylindrical shell is provided with the collecting tank of ring-type, the upper end open of described collecting tank and lower end closed, the outer wall of described cylindrical shell is provided with the middle melt outlet communicated with the bottom of described collecting tank, described middle melt outlet is connected with the entrance of middle melt Conveying pump, described middle melt Conveying delivery side of pump is connected with middle melt inlet, and described middle melt inlet to be positioned on cylinder body outer wall and to be positioned at the top of described cloth liquid dish.
2. fat polymerization two still system according to claim 1, it is characterized in that: the top of described cloth liquid dish is provided with film supplying tube dividing plate, the top of described film supplying tube dividing plate is provided with polymer reactor heating medium for heating pipe dividing plate, cylindrical shell laterally cuts off by described film supplying tube dividing plate and described polymer reactor heating medium for heating pipe dividing plate respectively, and the top of described polymer reactor heating medium for heating pipe dividing plate is provided with polymer reactor upper cover; The upper port of described film supplying tube is connected on the pore of described film supplying tube dividing plate, and the upper port of described polymer reactor heating medium for heating pipe is connected on the pore of described polymer reactor heating medium for heating pipe dividing plate; Described polymer reactor upper cover is connected with film supplying tube Heating medium, the barrel wall between described film supplying tube dividing plate and polymer reactor heating medium for heating pipe dividing plate is connected with film supplying tube heating agent and exports.
3. fat polymerization two still system according to claim 1, it is characterized in that: the barrel material that described cylinder inboard wall is provided with screw downward-extension distributes ring, the upper end that described barrel material distributes ring is positioned at below the outlet of described cloth liquid bath, the lower end that described barrel material distributes ring is positioned at above the upper port of described collecting tank, and described barrel material distribution ring is semi-circular cross-section and plane is connected on described cylinder inboard wall.
4. fat polymerization two still system according to claim 1, is characterized in that: the film supplying tube outer wall below described liquid distributing hole is evenly provided with at least one film supplying tube material and distributes ring, and the cross section that described film supplying tube material distributes ring is the little cydariform broad in the middle in two.
5. fat polymerization two still system according to claim 1, it is characterized in that: described esterification Prepolycondensating reactor comprises closed vertical tower body, be separated in esterification that under room and precondensation room in described vertical tower body by arc-shaped partition, in described esterification room barrel outside be provided with esterification heating jacket, under described precondensation room barrel outside be provided with precondensation heating jacket; In described esterification, the top of room is provided with room gaseous phase outlet and described material inlet in esterification, and the bottom centre of described arc-shaped partition is provided with nitrogen inlet, and in described esterification, the sidewall of room is provided with esterification material outlet; Under described precondensation, the bottom of room is connected with esterification material preheater, preheater charging aperture is provided with bottom the low head of described esterification material preheater, described esterification material outlet is connected with described preheater charging aperture with carboxylate discharge nozzle by esterifying liquid level control valve, described carboxylate discharge nozzle is connected with auxiliary agent import, and the preheater discharging opening of described esterification material preheater upper end is connected with the bottom inlet of room under described precondensation; Under described precondensation, the inner chamber of room is provided with multilayer tower tray from bottom to top, and described precondensation discharging opening is positioned on the top barrel of room under described precondensation, and the top of described precondensation discharging opening is provided with room vacuum orifice under precondensation.
6. fat polymerization two still system according to claim 5, it is characterized in that: in described esterification, the bottom centre of room is provided with and is horizontally disposed with and the cyclone agitator disk be centrosymmetric, described cyclone agitator disk is hollow cylinder plate, the bottom centre of described cyclone agitator disk is connected with described nitrogen inlet, the circumferential wall of described cyclone agitator disk is evenly distributed with multiple nitrogen jet mouth, the outside of each described nitrogen jet mouth is respectively equipped with the nitrogen water conservancy diversion arc that nitrogen is tangentially penetrated, the root of each described nitrogen water conservancy diversion arc is connected in the circumferential wall of described cyclone agitator disk.
7. fat polymerization two still system according to claim 6, it is characterized in that: in described esterification, the inner wall lower of room is provided with circumferentially and the external flow guiding cylinder of upper end open, described external flow guiding cylinder and esterification form esterification discharging annular groove between chamber interior walls, described external flow guiding cylinder is provided with external flow guiding cylinder material outlet and communicates with described esterification discharging annular groove, and described esterification material outlet communicates with the bottom of described esterification discharging annular groove; The inner chamber of described external flow guiding cylinder is provided with the inner draft tube of coaxial line with it, and the annular section between described inner draft tube and described external flow guiding cylinder is positioned at above the excircle of described cyclone agitator disk, and the upper port of described inner draft tube is lower than the upper port of external flow guiding cylinder; In described esterification, the inner chamber of room is provided with and expects to manage along the axis center extended downward in the middle part of inner draft tube, and the upper end of described center material pipe is connected with described material inlet; Between described external flow guiding cylinder and inner draft tube, annulus is provided with and organizes esterification heat(ing) coil more, often organizes heating medium for heating coil pipe and is respectively equipped with esterification heat(ing) coil Heating medium and the outlet of esterification heat(ing) coil heating agent.
8. fat polymerization two still system according to claim 5, it is characterized in that: described external flow guiding cylinder material outlet along the short transverse of described external flow guiding cylinder vertically to downward-extension, the inner chamber of described esterification discharging annular groove is provided with the radial diaphragm in room, and described external flow guiding cylinder material outlet and described esterification material outlet lay respectively at the both sides of the radial diaphragm in described upper room; The top of top tray is provided with discharging annular groove in room under precondensation, under described precondensation, the bottom of room discharging annular groove is connected on the barrel of room under described precondensation, under described precondensation, room discharging annular groove is provided with room flash mouth under the precondensation vertically extended, described precondensation discharging opening communicates with the bottom of room discharging annular groove under described precondensation, under described precondensation, the inner chamber of room discharging annular groove is provided with the radial diaphragm in room under precondensation, and under described precondensation, room flash mouth and described precondensation discharging opening lay respectively at the both sides of room radial direction diaphragm under described precondensation.
9. fat polymerization two still system according to claim 5, it is characterized in that: the material tedge described tower tray of each layer being evenly distributed with respectively multiple through tower tray, the top of each described material tedge is coated with the material deflector cup of coaxial line with it respectively, each described material deflector cup is fornix shape and lower port is connected on described tower tray, and the lower circumference of each described material deflector cup is evenly provided with deflector cup discharging opening.
10. fat polymerization two still system according to claim 8, it is characterized in that: under described precondensation, the top of room discharging annular groove is provided with foam trapping dish, the below of room vacuum orifice on the cross section that described foam trapping dish is horizontally set on room under described precondensation and under being positioned at described precondensation; The low head inner chamber of described esterification material preheater is respectively equipped with horizontally disposed material distribution plate, and described material distribution plate is evenly distributed with multiple material dispensing orifice.
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