CN105561905B - A kind of kettle system of fat polymerization two - Google Patents

A kind of kettle system of fat polymerization two Download PDF

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Publication number
CN105561905B
CN105561905B CN201610097833.3A CN201610097833A CN105561905B CN 105561905 B CN105561905 B CN 105561905B CN 201610097833 A CN201610097833 A CN 201610097833A CN 105561905 B CN105561905 B CN 105561905B
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precondensation
esterification
cylinder
room
polymer reactor
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CN105561905A (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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Yangzhou Huitong Chemical Polytron Technologies Inc
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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 present invention relates to a kind of kettle system of fat polymerization two, the precondensation discharging opening for being esterified Prepolycondensating reactor is connected by precondensation fluid level control valve or precondensation melt conveying pump with the polymer reactor charging aperture without stirring polymer reactor.The top of polymer reactor inner chamber is provided with cloth liquid disk, film supplying tube is provided with liquid distributing hole, falling liquid film tube cavity is plugged with heating medium for heating pipe, cylinder external wall of upper portion is provided with polymer reactor charging aperture and vacuum orifice, the bottom of polymer reactor is provided with discharging spiral and polymer discharge mouthful, cylinder inboard wall position corresponding with polymer reactor charging aperture is provided with ring-type cloth liquid bath, and uniform annular slot is left in the lower end of cloth liquid bath;The lower inner wall of cylinder is provided with collecting tank;Cylinder body outer wall is provided with the middle melt outlet communicated with collecting tank, and middle melt outlet passes through middle melt conveying pump and is connected with middle melt inlet, and middle melt inlet is located at the top of cloth liquid disk.The kettle system architecture of fat polymerization two is compact, and floor space is small, and production efficiency is high.

Description

A kind of kettle system of fat polymerization two
Technical field
The present invention relates to a kind of kettle system of fat polymerization two, belong to polyester producing process field.
Background technology
In the prior art, during production of polyester esterification and polycondensation reaction is general in separate reaction tower or reaction Carried out in kettle, such as the Chinese invention patent of Publication No. CN101618304B, a kind of esterifier is disclosed, by polylith column plate Composition, all installs a downspout and a riser on every block of column plate, riser connects rotatable gas distributor, gas Distributor is made up of air entraining pipe, fan blades and nozzle.Every block of column plate all retains the liquid of certain liquid level, there is solid catalysis in liquid Agent.Liquid phase is the component containing carboxylic acid, next block of column plate is flowed to by one block of esterification column plate downwards in the reactor, with the alcohol for rising Steam counter-flow reacts.
A kind of Chinese invention patent of Publication No. CN2741645, the polycondensation disclosed in polycondensation reaction device field is anti- Tower is answered, including the double Shell being 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 import and export of chuck is connected, steam outlet port, charging aperture and the discharging of inner casing intracoelomic cavity are communicated with double Shell Mouthful, the double Shell is uprightly set, and charging aperture is arranged at double Shell top and stretches into inner housing, and discharging opening is arranged at double The bottom of layer housing, is provided with some horizontally disposed tower trays between charging aperture and discharging opening, the tower tray includes housing, outer inframe It is provided with some material leakage passages.Traditionally esterification and polycondensation reaction is divided into two reactors and carries out, and structure is not compact enough, takes up an area Area is big, low production efficiency.
Traditional polymer reactor includes the cylinder of vertical setting and closed at both ends, and the top of polymer reactor inner chamber is provided with Horizontal material distribution plate, material distribution plate is provided with material distribution hopper, and closed at both ends is provided with material distribution hopper Film supplying tube and gap uniformity between the two, film supplying tube extends straight down and upper end is stretched out outside the top of polymer reactor, drop The inner chamber of membrane tube is provided with heating medium for heating pipe, and 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 mouthful, and the periphery of polymer reactor is provided with heating jacket.
After PET melt enters polymer reactor inner chamber, fall on material distribution plate, the material distribution from material distribution plate Gap between funnel and film supplying tube is flowed downward out, and wall built-up falling liquid film, the thermal medium in film supplying tube are formed in the outer wall of film supplying tube Heating under, after melt completes polymerization, fall in polymer reactor bottom, then from the polymer discharge mouthful stream of polymer reactor bottom Go out.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 for being heated is small, and it is anti-to be only once polymerized Should, reaction speed is slow, low production efficiency;The small molecule for producing is reacted easily in the carbonization of kettle wall, is fallen into the middle of material, produce stain Material, it is often necessary to which kettle is washed in parking, and unstable product quality, the cycle of operation is short.
The content of the invention
It is an object of the present invention to overcome problems of the prior art, there is provided a kind of kettle system of fat polymerization two, knot Structure is compact, and production efficiency is high.
To solve above technical problem, a kind of kettle system of fat polymerization of the invention two, including esterification Prepolycondensating reactor With without stirring polymer reactor, the esterification Prepolycondensating reactor is provided with material inlet and precondensation discharging opening, described without stirring Polymer reactor is provided with polymer reactor charging aperture and polymer discharge mouthful, and the precondensation discharging opening passes through precondensation liquid level control Valve processed or precondensation melt conveying pump are connected with precondensation discharge nozzle, and the precondensation discharge nozzle feeds with the polymer reactor Mouth is connected, and described to include the cylinder of vertical setting and closed at both ends without stirring polymer reactor, the top of cylinder lumen is provided with Cloth liquid disk that is horizontal and laterally separating cylinder, the cloth liquid disk is provided with up big and down small liquid distributing hole, in the liquid distributing hole Film supplying tube and both coaxial lines are provided with, the film supplying tube extends straight down, and the inner chamber of the film supplying tube is plugged with polymerisation Device heating medium for heating pipe, the external wall of upper portion of the cylinder is provided with polymer reactor vacuum orifice and the polymer reactor charging aperture, The lower end of the cylinder is provided with conical head, and the lower end of the conical head is provided with discharging spiral, and the polymer discharge mouthful is located at institute State the lower end of discharging spiral;The periphery of the cylinder is provided with polymer reactor chuck, and the periphery of the conical head is provided with conical head Chuck, the polymer reactor charging aperture is located at the lower section of the cloth liquid disk, the inwall of the cylinder and the polymer reactor The corresponding position of charging aperture is provided with the cloth liquid bath of ring-type, and uniform ring-type is left between the lower end of the cloth liquid bath and cylinder inboard wall Gap;The lower inner wall of the cylinder is provided with the collecting tank of ring-type, the upper end open and lower end closed of the collecting tank;The cylinder The outer wall of body is provided with the middle melt outlet communicated with the bottom of the collecting tank, the middle melt outlet and middle melt The entrance connection of delivery pump, the outlet of the middle melt conveying pump is connected with middle melt inlet, the middle melt inlet On cylinder body outer wall and positioned at the top of the cloth liquid disk.
Relative to prior art, the present invention achieves following beneficial effect:When using precondensation fluid level control valve, preshrunk Poly- melt enters polymer reactor charging aperture by potential difference;When using precondensation melt conveying pump, by precondensation melt conveying Pump is conveyed to polymer reactor charging aperture.Precondensation melt enters cloth liquid bath from polymer reactor charging aperture, with cloth liquid bath in cylinder It is uniformly distributed on the circumference of internal wall, is then flowed out from the annular slot of cloth liquid bath lower end, forms uniform on cylinder inboard wall Falling liquid film, in flow process, in the chuck under the heating of heating agent, melt heats up and is able to prepolymerization as melt in the middle of prepolymerization, Then flow into the collecting tank of cylinder inboard wall bottom, then flowed out from middle melt outlet, then be pumped into by middle melt conveying The middle melt inlet on polymer reactor top, after entering polymer reactor inner chamber from middle melt inlet, falls in cloth liquid disk On, the gap between liquid distributing hole and film supplying tube from cloth liquid disk is flowed downward out, and wall built-up drop is formed again in the outer wall of film supplying tube Film, in the film supplying tube under the heating of thermal medium, melt is further polymerized completion in the middle of prepolymerization, from polymer reactor bottom Polymer discharge mouthful outflow.The polymer reactor is used without stirring structure, and power consumption and fault rate are low;Adopted in polymer reactor inner chamber With ring-type cloth liquid bath cloth liquid, the falling liquid film of formation is uniform, and is polymerized twice in polymer reactor inner chamber, improves reaction effect Rate;During reaction and discharging, it is evacuated by polymer reactor vacuum orifice, polymer reactor inner chamber remains at vacuum State, does not result in melt degraded, product with stable quality.
As improvement of the invention, film supplying tube dividing plate, the top of the film supplying tube dividing plate are provided with above the cloth liquid disk Polymer reactor heating medium for heating pipe dividing plate is provided with, the film supplying tube dividing plate and the polymer reactor heating medium for heating pipe dividing plate are distinguished Cylinder is laterally separated, polymer reactor upper cover is provided with above the polymer reactor heating medium for heating pipe dividing plate;The drop The upper port of membrane tube is connected on the pore of the film supplying tube dividing plate, the upper port connection of the polymer reactor heating medium for heating pipe On the pore of the polymer reactor heating medium for heating pipe dividing plate;Film supplying tube heating agent is connected with the polymer reactor upper cover Import, is connected with film supplying tube heating agent and goes out on the barrel wall between the film supplying tube dividing plate and polymer reactor heating medium for heating pipe dividing plate Mouthful.Thermal medium such as conduction oil enters polymer reactor upper cover and polymer reactor heating medium for heating from film supplying tube Heating medium Oil suction chamber between pipe dividing plate, it is then directly lower to polymer reactor heating medium for heating ttom of pipe along polymer reactor heating medium for heating pipe Portion, the ring-type being upwardly into after outflow polymer reactor heating medium for heating pipe between film supplying tube and polymer reactor heating medium for heating pipe is empty Chamber, it is up along the ring cavity, enter film supplying tube dividing plate and polymer reactor heating medium for heating pipe dividing plate from the upper port of film supplying tube Between go out oil pocket, finally from film supplying tube heating agent export flow out.Temperature is relatively low when material has just enter into liquid distributing hole, forms edge after falling liquid film Film supplying tube flows downward, and is constantly heated by heating agent in film supplying tube, and temperature gradually rises, material when reaching falling liquid film bottom of the tube Temperature reaches highest.Temperature highest heating agent is lower to falling liquid film bottom of the tube first, because the periphery of polymer reactor heating medium for heating pipe It is the heating agent of return, temperature is higher, along the descending heating agent thermal loss very little of polymer reactor heating medium for heating pipe;Return is up Due to constantly carrying out heat release to material falling liquid film, temperature is gradually reduced heating agent.Therefore the temperature of the outer material of film supplying tube from top to bottom by Gradually it is incremented by, the heat medium temperature in film supplying tube gradually successively decreases from bottom to top, the minimum material of the temperature heating agent relatively low with temperature is carried out Heat exchange, temperature highest material is exchanged heat with temperature highest heating agent, and heat exchange both sides remain the larger temperature difference, heat exchange effect Rate is high.
As a further improvement on the present invention, the cylinder inboard wall is provided with the barrel material distribution ring of downward spiral extension, The upper end of the barrel material distribution ring is located at the outlet lower section of the cloth liquid bath, and the lower end of the barrel material distribution ring is located at The upper port top of the collecting tank, the barrel material distribution ring is for semi-circular cross-section and plane is connected to the cylinder inboard wall On.Melt flows out from the annular slot of cloth liquid bath lower end, flows downward to be formed after falling liquid film, it is necessary to cross multiple tracks half along cylinder inboard wall The barrel material distribution ring of circular cross-section, is blocked when barrel material distribution ring is crossed, and makes cylinder inboard wall whole circumference side To and short transverse falling liquid film thickness it is more uniform;Semi-circular cross-section surface is smooth so that melt flows are highly uniform gentle, and In the absence of material dead angle, it is to avoid material is stagnated causes overheat.
As a further improvement on the present invention, the falling liquid film pipe outer wall below the liquid distributing hole is uniformly provided with least one falling liquid film Pipe material distribution ring, the section of the film supplying tube material distribution ring is in the small cydariform broad in the middle in two.Middle melt is from cloth liquid disk On liquid distributing hole and film supplying tube between gap flow downward out, after the outer wall of film supplying tube forms wall built-up falling liquid film again, downward Need to cross the film supplying tube material distribution ring of multiple tracks cydariform in flow process, hindered when film supplying tube material distribution ring is crossed It is stagnant, make the falling liquid film thickness of falling liquid film pipe outer wall whole circumference direction and short transverse more uniform;The table of film supplying tube material distribution ring Face smooth arc transition causes that melt flows are highly uniform gentle, and in the absence of material dead angle, it is to avoid material is stagnated causes overheat.
As a further improvement on the present invention, the esterification Prepolycondensating reactor includes the vertical tower body of closing, described vertical It is separated into by arc-shaped partition in formula tower body and is esterified room under upper chamber and precondensation, the barrel of the esterification upper chamber is externally provided with esterification heating Chuck, the barrel of room is externally provided with precondensation heating jacket under the precondensation;Esterification upper chamber is provided with the top of the esterification upper chamber Gaseous phase outlet and the material inlet, the bottom centre of the arc-shaped partition are provided with nitrogen inlet, the side wall of the esterification upper chamber It is provided with esterification material outlet;The bottom of room is connected with esterification material preheater, the esterification material preheater under the precondensation Low head bottom be provided with preheater charging aperture, the esterification material outlet is by being esterified fluid level control valve and carboxylate discharge nozzle It is connected with the preheater charging aperture, auxiliary agent import is connected with the carboxylate discharge nozzle, on the esterification material preheater The preheater discharging opening at end is connected with the bottom inlet of room under the precondensation;The inner chamber of room sets from bottom to top under the precondensation There is a multilayer tower tray, the precondensation discharging opening is located under the precondensation on the top barrel of room, the precondensation discharging opening Top is provided with room vacuum orifice under precondensation.Enter esterification upper chamber, nitrogen from material inlet after PTA powders and ethylene glycol mixing mashing Gas enters esterification upper chamber from the nitrogen inlet of arc-shaped partition bottom, and material is stirred is well mixed it, in esterification upper chamber Hot environment under, there is esterification in PTA powders and ethylene glycol, the operating pressure for being esterified upper chamber is 0.5~2bar(Gauge pressure), The gaseous substance that esterification is produced passes through from the gaseous phase outlet discharge of esterification upper chamber, esterification material from esterification material outlet discharge Esterification fluid level control valve enters carboxylate discharge nozzle, and auxiliary agent is added in carboxylate discharge nozzle by auxiliary agent import;In potential difference and In the presence of pressure difference, esterification material and auxiliary agent enter preheater charging aperture, in material preheater is esterified, excessive second in auxiliary agent Glycol gasification produces bubble, and bubble is from bottom to top moved to material with motive force, while playing stirring action;Esterification material is added Room under precondensation is upwardly into after heat, proceeds partial esterification reaction, while into polycondensation process;The preshrunk of room under precondensation Poly- lower room vacuum orifice is located at topmost, and more higher toward upper strata vacuum, the vacuum in ceiling portion is 1~10kpa under precondensation (Absolute pressure), material progressively carries out polymerisation when through tower tray layer by layer, material is polymerized during from bottom to top Degree is incrementally increased, and is finally discharged from precondensation discharging opening.The reactor will be esterified room and precondensation room is connected as a single entity, and structure is tight Gather, floor space is small, heat loss is few, room under can flowing to precondensation from upper chamber is esterified without extra power material, mechanical is stirred Device is mixed, energy consumption has been saved, fault rate is reduced, production efficiency is improve.
As a further improvement on the present invention, the bottom centre of the esterification upper chamber is provided with horizontally disposed and is centrosymmetric Cyclone agitator disk, the cyclone agitator disk is hollow cylinder plate, bottom centre and the nitrogen of the cyclone agitator disk Import is connected, and multiple nitrogen jets mouthful are evenly distributed with the circumferential wall of the cyclone agitator disk, each nitrogen jet mouthful Outside is respectively equipped with the nitrogen water conservancy diversion arc for making nitrogen tangentially project, and the root of each nitrogen water conservancy diversion arc connects respectively It is connected in the circumferential wall of the cyclone agitator disk.Nitrogen enters the inner chamber of cyclone agitator disk from the bottom centre of cyclone agitator disk, Sprayed from each nitrogen jet mouthful, by the water conservancy diversion of nitrogen water conservancy diversion arc, nitrogen is along nitrogen water conservancy diversion arc tip circle everywhere Tangential direction project, esterification upper chamber bottom formed level be vortexed, fully material can be stirred, nitrogen project Also to move upwards afterwards and secondary agitation is formed to material, it is ensured that material is thoroughly mixed uniformly.
As a further improvement on the present invention, the inner wall lower of the esterification upper chamber is provided with circumferentially and upper end open External flow guiding cylinder, esterification discharging annular groove is formed between the external flow guiding cylinder and the upper chamber interior walls of esterification, the external flow guiding cylinder is provided with External flow guiding cylinder material outlet is communicated with the esterification discharging annular groove, the bottom for being esterified material outlet and the esterification discharging annular groove Portion communicates;The inner chamber of the external flow guiding cylinder is provided with the inner draft tube of line coaxially therewith, the inner draft tube and the external flow guiding cylinder Between annular section be located at the excircle top of the cyclone agitator disk, the upper port of the inner draft tube is less than external flow guiding cylinder Upper port;The inner chamber of the esterification upper chamber is provided with and extends downward center expects pipe in the middle part of inner draft tube along axis, it is described in The upper end of heart expects pipe is connected with the material inlet;Annulus is provided with multigroup esterification between the external flow guiding cylinder and inner draft tube Heating coil, every group of heating medium for heating coil pipe is respectively equipped with esterification heating coil Heating medium and the heating agent outlet of esterification heating coil. The nitrogen that cyclone agitator disk is projected makes the material of esterification upper chamber bottom form strong circulation, in the hot right of nitrogen and heating coil Under stream double action, annulus of the material between inner draft tube and external flow guiding cylinder is moved upwards;Thing inside inner draft tube Material flows downward, and forms the state of inside and outside stream circulation, after new material is flowed downward out from the lower port of center expects pipe, that is, is involved in Stirred in stream circulation;At high temperature there is esterification in PTA powders with ethylene glycol, as new material constantly enters Enter, the material for having reacted enters esterification discharging annular groove from the external flow guiding cylinder material outlet of external flow guiding cylinder, in heating jacket is esterified Continue to react thorough during being flowed under the heating of heating agent, finally from the esterification material outlet discharge of esterification discharging ring trench bottom. PTA powders and ethylene glycol between external flow guiding cylinder and inner draft tube in annulus while stir, while being esterified kettle heating dish Pipe is heated, and can be needed to determine the group number of the esterifying kettle heating coil of input heating according to technique.
As a further improvement on the present invention, the external flow guiding cylinder material outlet is erected along the short transverse of the external flow guiding cylinder To extending downwardly, the inner chamber of the esterification discharging annular groove is provided with upper chamber radial direction diaphragm, the external flow guiding cylinder material outlet with The esterification material outlet is respectively positioned at the both sides of the upper chamber radial direction diaphragm;It is provided with precondensation above top tray Room is discharged annular groove, and the bottom of room discharging annular groove is connected under the precondensation on the barrel of room under the precondensation, the preshrunk Poly- lower room discharging annular groove is provided with room flash mouthful, the precondensation discharging opening and the precondensation under vertically extending precondensation The bottom of lower room discharging annular groove communicates, under the precondensation inner chamber of room discharging annular groove be provided with precondensation room radial direction water conservancy diversion every Plate, room flash mouthful is located at room radial direction diaphragm under the precondensation with the precondensation discharging opening respectively under the precondensation Both sides.Upper chamber radial direction diaphragm separates material outlet is esterified with external flow guiding cylinder material outlet, can prevent from being esterified discharging ring There is short stream in the material in groove, material is had maximum stroke in esterification discharging annular groove, and material enters esterification discharging annular groove Afterwards in the form of laminar flow, along tower body inner wall surrounding one week, material continued to be esterified heating jacket during advance and heats, most Afterwards from esterification material outlet outflow, the structure extends heat time of the material in esterification discharging annular groove.Room footpath under precondensation Room flash under precondensation mouthful is separated with precondensation discharging opening to diaphragm, can prevent room under precondensation from discharging in annular groove There is short stream in material, material is had maximum stroke in discharging annular groove in room under precondensation, and material goes out into room under precondensation In the form of laminar flow after material annular groove, along tower body inner wall surrounding one week, material continued by precondensation heating folder during advance Set heating, finally flows out from precondensation discharging opening, when the structure extends heating of the material in discharging annular groove in room under precondensation Between.
As a further improvement on the present invention, the material of multiple insertion tower trays is respectively uniformly distributed on each layer tower tray Tedge, is covered each by the material deflector cup of line coaxially therewith, each material baffling above each material tedge It is that fornix shape and lower port are connected on the tower tray to cover, and deflector cup is uniformly provided with the lower circumference of each material deflector cup Discharging opening.Material is advanced into the inner chamber of material deflector cup from material tedge, and then baffling is downwards from material deflector cup bottom Deflector cup discharging opening outflow on circumference.Due to the swabbing action and material of room vacuum orifice under room top precondensation under precondensation Polycondensation process, form air cavity, the vacuum in most last layer material deflector cup air cavity at the top of each layer of material deflector cup Highest, more down the vacuum in material deflector cup air cavity progressively successively decrease, material from bottom to top passes sequentially through each layer tower tray and thing Polymerisation is progressively carried out during material deflector cup, material degree of polymerization during from bottom to top is incrementally increased.
As a further improvement on the present invention, foam trapping disk, institute are provided with the precondensation above room discharging annular groove Foam trapping disk is stated to be horizontally set under the precondensation on the cross section of room and the room vacuum orifice under the precondensation Lower section;The low head inner chamber of the esterification material preheater is respectively equipped with horizontally disposed material distribution plate, the material distribution Multiple material dispensing orifices are evenly distributed with disk.A large amount of bubbles, foam trapping disk can be produced in polymerization process can prevent preshrunk The bubble of poly- lower room enters under the precondensation of top room vacuum meter interface under room vacuum orifice and precondensation.Esterification material and auxiliary agent By after numerous material dispensing orifices of material distribution plate, can more uniformly enter each heat exchanging pipe of top.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description, accompanying drawing only provide with reference to Illustrate to use, be not used to the limitation present invention.
Fig. 1 is the schematic diagram of kettle system the first implementation method of fat polymerization of the present invention two.
Fig. 2 is the schematic diagram of second implementation method of kettle system of fat polymerization of the present invention two.
Fig. 3 is the structural representation of polymer reactor of the present invention.
Fig. 4 is the enlarged drawing at A positions 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 positions 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. upper chamber is esterified;1a. material inlets;1b. is esterified upper chamber gaseous phase outlet;1c. nitrogen inlets;The outer water conservancy diversion of 1d. Cylinder;1d1. external flow guiding cylinder material outlets;1e. esterification discharging annular grooves;1e1. upper chamber radial direction diaphragms;1f. is esterified material outlet; 1g. inner draft tubes;1h. cyclone agitator disks;1h1. nitrogen jets mouthful;1h2. nitrogen water conservancy diversion arcs;1j. is esterified upper chamber liquid level gauge Interface;1k. is esterified upper chamber pressure gauge connection;1m. is esterified upper chamber Heating medium;1n. esterification upper chamber heating agent outlets;1p. esterifications add Hot coil.
2. room under precondensation;2a. tower trays;2a1. material tedges;2a2. material deflector cups;2a3. deflector cup discharging openings; Discharging annular groove in room under 2b. precondensations;Room flash mouthful under 2b1. precondensations;Radial direction diaphragm in room under 2b2. precondensations;2c. preshrunks Poly- discharging opening;2d. foams trap disk;Room vacuum orifice under 2e. precondensations;Room interface of the level gauge under 2f. precondensations;2g. preshrunks Poly- lower room vacuum meter interface;Room Heating medium under 2h. precondensations;Heating agent outlet in room under 2j. precondensations.
3. material preheater is esterified;3a. preheater charging apertures;3b. preheater discharging openings;3c. preheater Heating mediums; 3d. preheaters heating agent is exported;3e. material distribution plates;3e1. material dispensing orifices.
B1. precondensation melt conveying pump;G1. carboxylate discharge nozzle;G1a. auxiliary agent import;G2. precondensation discharge nozzle;V1. Esterification fluid level control valve;V2. precondensation fluid level control valve.
4. without stirring polymer reactor;401a. polymer reactor charging apertures;401b. polymer reactor vacuum orifices; Melt inlet in the middle of 401c.;Melt outlet in the middle of 401d.;401e. polymer reactor heating medium for heating pipe dividing plates;401f. film supplying tubes Dividing plate;402. cloth liquid disks;402a. liquid distributing holes;403. film supplying tubes;403a. film supplying tube material distribution rings;404. cloth liquid baths;405. Collecting tank;406. middle melt conveying pumps;407. polymer reactor chucks;407a. polymer reactor chuck Heating mediums; 407b. polymer reactor chucks heating agent is exported;408a. film supplying tube Heating mediums;408b. film supplying tubes heating agent is exported;409a. tapers Head chuck Heating medium;409b. conical head chucks heating agent is exported;410. discharging spirals;410a. polymer discharges mouthful;411. gather Close reactor heating medium for heating pipe;412. barrel material distribution rings;413. collecting tank interface of the level gauge;414. conical head liquid level gauges connect Mouthful.
Specific embodiment
Shown in Fig. 1, the kettle system of fat polymerization of the invention two includes esterification Prepolycondensating reactor and without stirring polymerisation Device 4, esterification Prepolycondensating reactor is provided with material inlet 1a and precondensation discharging opening 2c, and polymerization is provided with without stirring polymer reactor 4 Reactor feed mouthful 401a and polymer discharge mouthful 410a, precondensation discharging opening 2c pass through precondensation fluid level control valve V2 and preshrunk Poly- discharge nozzle G2 is connected, and precondensation discharge nozzle G2 is connected with polymer reactor charging aperture 401a.
Shown in Fig. 2, the kettle system of fat polymerization of the invention two includes esterification Prepolycondensating reactor and without stirring polymerisation Device 4, esterification Prepolycondensating reactor is provided with material inlet 1a and precondensation discharging opening 2c, and polymerization is provided with without stirring polymer reactor 4 Reactor feed mouthful 401a and polymer discharge mouthful 410a, precondensation discharging opening 2c pass through precondensation melt conveying pump B1 and preshrunk Poly- discharge nozzle G2 is connected, and precondensation discharge nozzle G2 is connected with polymer reactor charging aperture 401a.
As shown in Figure 3 and Figure 4, the cylinder of vertical setting and closed at both ends, cylinder lumen are included without stirring polymer reactor 4 Top be provided with horizontal and by the cloth liquid disk 402 of the horizontal cut-off of cylinder, cloth liquid disk 402 is provided with liquid distributing hole 402a, liquid distributing hole Film supplying tube 403 and both coaxial lines are provided with 402a.Liquid distributing hole 402a is up big and down small infundibulate, is easy to enough material stream In entering 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 is vertical Extend downwardly, the inner chamber of film supplying tube 403 is plugged with polymer reactor heating medium for heating pipe 411, the cylinder without stirring polymer reactor 4 External wall of upper portion is provided with polymer reactor charging aperture 401a and polymer reactor vacuum orifice 401b, without stirring polymer reactor 4 Lower end is provided with conical head, and the lower end of conical head is provided with discharging spiral 410, and the lower end of the spiral 410 that discharges is provided with polymer discharge mouthful 410a。
Cylinder periphery without stirring polymer reactor 4 is provided with polymer reactor chuck 407, polymer reactor chuck 407 Bottom 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 exports 407b.Heating agent enters in polymer reactor chuck 407 from polymer reactor chuck Heating medium 407a, then from poly- Close the outlet 407b outflows of reactor jacket heating agent.
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, the top of conical head chuck is provided with conical head chuck heating agent outlet 409b.Heating agent is from conical head chuck Heating medium 409a Into in conical head chuck, then from the outlet 409b outflows of conical head chuck heating agent.
Polymer reactor charging aperture 401a be located at cloth liquid disk 402 lower section, without stirring polymer reactor 4 cylinder inboard wall with The corresponding positions of polymer reactor charging aperture 401a are provided with the cloth liquid bath 404 of ring-type, the lower end and cylinder inboard wall of cloth liquid bath 404 it Between leave uniform annular slot;Lower inner wall without stirring polymer reactor 4 is provided with the collecting tank 405 of ring-type, collecting tank 405 Upper end open and lower end closed;Outer wall without stirring polymer reactor 4 is provided with the centre communicated with the bottom of collecting tank 405 Melt outlet 401d, middle melt outlet 401d are connected with the entrance of middle melt conveying pump 406, middle melt conveying pump 406 Outlet be connected with centre melt inlet 401c, middle melt inlet 401c be located at cylinder body outer wall on and positioned at cloth liquid disk 402 Top.
Middle melt outlet 401d and centre melt inlet 401c can be uniform on the circumference without stirring polymer reactor 4 It is provided with one group, two groups or more than three groups.
Multiple liquid distributing hole 402a can be provided with cloth liquid disk 402, the center of each liquid distributing hole 402a is respectively equipped with film supplying tube 403.Film supplying tube 403 is at least provided with one group, and every group is equipped with polymer reactor heating medium for heating pipe 411.
The top of cloth liquid disk 402 is provided with film supplying tube dividing plate 401f, and polymer reactor is provided with above film supplying tube dividing plate 401f Heating medium for heating pipe dividing plate 401e, polymer reactor heating medium for heating pipe dividing plate 401e and film supplying tube dividing plate 401f are respectively by cylinder transverse direction Cut-off, polymer reactor upper cover is provided with above polymer reactor heating medium for heating pipe dividing plate 401e;The upper port of film supplying tube 403 It is connected on the pore of film supplying tube dividing plate 401f, the upper port of polymer reactor heating medium for heating pipe 411 is connected to polymer reactor On the pore of heating medium for heating pipe dividing plate 401e;Film supplying tube Heating medium 408a, film supplying tube are connected with polymer reactor upper cover Film supplying tube heating agent outlet 408b is connected with barrel wall between dividing plate 401f and polymer reactor heating medium for heating pipe dividing plate 401e.
Polymer reactor vacuum orifice 401b is located at the lower section of cloth liquid disk 402, during reaction and discharging, by polymerization Reactor vacuum orifice 401b is evacuated, and polymer reactor inner chamber remains at vacuum state.
Position corresponding with the lower end of collecting tank 405 is provided with collecting tank interface of the level gauge 413, conical head on polymer reactor Lower end be 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 on the circumference of cylinder inboard wall It is uniformly distributed, is then flowed out from the annular slot of the lower end of cloth liquid bath 404, uniform falling liquid film is formed on cylinder inboard wall, in flowing During, in the polymer reactor chuck under the heating of heating agent, melt heats up and is able to prepolymerization as melt in the middle of prepolymerization, so Flow into afterwards in the collecting tank 405 of cylinder inboard wall bottom, then flowed out from middle melt outlet 401d, then by middle melt conveying pump The middle melt inlet 401c on 406 feeding polymer reactor tops, polymer reactor inner chamber is entered from middle melt inlet 401c Afterwards, fall on cloth liquid disk 402, the gap between liquid distributing hole 402a and film supplying tube 403 from cloth liquid disk 402 flows downward out, The outer wall of film supplying tube 403 forms wall built-up falling liquid film again, in the film supplying tube 403 under the heating again of thermal medium, in the middle of prepolymerization Melt is further polymerized completion, and discharging spiral 410 is entered from the conical head of polymer reactor bottom, then under discharging spiral 410 The polymer discharge mouthful 410a discharges at end.The esterification yield of polymer discharge mouthful 410a is more than 99%, and the degree of polymerization is more than 100.
Thermal medium such as conduction oil enters polymer reactor upper cover and polymerisation from film supplying tube Heating medium 408a Oil suction chamber between device heating medium for heating pipe dividing plate 401e, it is then directly lower anti-to polymerization along polymer reactor heating medium for heating pipe 411 The bottom of device heating medium for heating pipe 411 is answered, film supplying tube 403 is upwardly into after outflow polymer reactor heating medium for heating pipe 411 and is polymerized instead The ring cavity between device heating medium for heating pipe 411 is answered, it is up along the ring cavity, enter falling liquid film from the upper port of film supplying tube 403 Go out oil pocket between pipe dividing plate 401f and polymer reactor heating medium for heating pipe dividing plate 401e, finally export 408b from film supplying tube heating agent Outflow.
Temperature is relatively low when material has just enter into liquid distributing hole 402a, is flowed downward along film supplying tube 403 after forming falling liquid film, is constantly subject to The heating of heating agent in film supplying tube 403, temperature continues to raise, and the temperature of material reaches highest when reaching 403 bottom of film supplying tube.And it is warm Degree highest heating agent is lower to the bottom of film supplying tube 403 first, because the periphery of polymer reactor heating medium for heating pipe 411 is the heat of return Matchmaker, temperature is higher, along the descending heating agent thermal loss very little of polymer reactor heating medium for heating pipe 411;The up heating agent of return by In constantly heat release is carried out to material falling liquid film, temperature is gradually reduced.Therefore the temperature of the outer material of film supplying tube is gradually incremented by from top to bottom, Heat medium temperature in film supplying tube gradually successively decreases from bottom to top, and the relatively low material of the temperature heating agent relatively low with temperature is exchanged heat, temperature Degree highest material is exchanged heat with temperature highest heating agent, and heat exchange both sides remain the larger temperature difference, and heat exchange efficiency is high.Should Polymer reactor uses the cloth liquid of ring-type cloth liquid bath 404 in polymer reactor inner chamber, outer using liquid distributing hole 402a cloth in film supplying tube 403 Liquid, the falling liquid film of formation is all visibly homogeneous, and is polymerized twice in polymer reactor inner chamber, increases heat exchange area, improves Reaction efficiency.
Cylinder inboard wall is provided with the barrel material distribution ring 412 of downward spiral extension, the upper end position of barrel material distribution ring 412 In the outlet lower section of cloth liquid bath 404, the lower end of barrel material distribution ring 412 is located at the upper port top of collecting tank 405, barrel thing Material distribution ring 412 is that semi-circular cross-section and plane are connected on cylinder inboard wall.Annular slot stream of the melt from the lower end of cloth liquid bath 404 Go out, flow downward to be formed after falling liquid film, it is necessary to cross the barrel material distribution ring 412 of multiple tracks semi-circular cross-section along cylinder inboard wall, Blocked when crossing barrel material distribution ring 412, made the falling liquid film thickness of cylinder inboard wall whole circumference direction and short transverse more Plus it is uniform;Semi-circular cross-section surface is smooth so that melt flows are highly uniform gentle, and in the absence of material dead angle, it is to avoid material stops It is stagnant to cause overheat.
The outer wall of film supplying tube 403 below liquid distributing hole is uniformly provided with least one film supplying tube material distribution ring 403a, film supplying tube The section of material distribution ring 403a is in the small cydariform broad in the middle in two.Liquid distributing hole and falling liquid film of the middle melt from cloth liquid disk 402 Gap between pipe 403 flows downward out, after the outer wall of film supplying tube 403 forms wall built-up falling liquid film again, during flowing downward Need to cross the film supplying tube material distribution ring 403a of multiple tracks cydariform, blocked when film supplying tube material distribution ring 403a is crossed, Make the falling liquid film thickness of falling liquid film pipe outer wall whole circumference direction and short transverse more uniform;The table of film supplying tube material distribution ring 403a Face smooth arc transition causes that melt flows are highly uniform gentle, and in the absence of material dead angle, it is to avoid material is stagnated causes overheat.
As shown in Fig. 5 to Figure 10, esterification Prepolycondensating reactor includes the vertical tower body of closing, in vertical column body by arc every Plate is separated into room 2 under esterification upper chamber 1 and precondensation, and the barrel for being esterified upper chamber 1 is externally provided with esterification heating jacket, room 2 under precondensation Barrel be externally provided with precondensation heating jacket;The top for being esterified upper chamber 1 is provided with material inlet 1a and esterification upper chamber gaseous phase outlet 1b, The bottom centre of arc-shaped partition is provided with nitrogen inlet 1c, and the side wall for being esterified upper chamber 1 is provided with esterification material outlet 1f, is esterified upper chamber 1 Top be provided with esterification upper chamber pressure gauge connection 1k.
The bottom of room 2 is connected with esterification material preheater 3 under precondensation, and the low head bottom for being esterified material preheater 3 sets There is preheater charging aperture 3a, esterification material outlet 1f is by being esterified fluid level control valve V1 or precondensation melt conveying pump B1 with esterification Thing discharge nozzle G1 is connected, and carboxylate discharge nozzle G1 is connected with preheater charging aperture 3a, and auxiliary agent is connected with carboxylate discharge nozzle G1 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.
The inner chamber of room 2 is provided with multilayer tower tray 2a from bottom to top under precondensation, and the top barrel of room 2 is provided with pre- under precondensation Polycondensation discharging opening 2c, precondensation discharging opening 2c pass through precondensation fluid level control valve V2 or precondensation melt conveying pump B1 and precondensation Discharge nozzle G2 is connected, and is provided with precondensation that room vacuum meter connects under room vacuum orifice 2e and precondensation above precondensation discharging opening 2c Mouth 2g.
Enter esterification upper chamber 1 from material inlet 1a after PTA powders and ethylene glycol mixing mashing, nitrogen is from arc-shaped partition bottom Nitrogen inlet 1c enter esterification upper chamber 1, material is stirred make its be well mixed, esterification upper chamber 1 hot environment under, There is esterification in PTA powders, the operating pressure for being esterified upper chamber 1 is 0.5~2bar with ethylene glycol(Gauge pressure), esterification generation Gaseous substance from esterification upper chamber gaseous phase outlet 1b discharge, esterification material from the 1f discharges of esterification material outlet, by being esterified liquid level Control valve V1 enters carboxylate discharge nozzle G1, and auxiliary agent is added in carboxylate discharge nozzle G1 by auxiliary agent import G1a.In potential difference and In the presence of pressure difference, esterification material and auxiliary agent enter preheater charging aperture 3a, excessive in auxiliary agent in material preheater 3 is esterified Ethylene glycol gasification produce bubble, bubble is from bottom to top moved to material with motive force, while playing stirring action.Esterification material Room 2 under precondensation is upwardly into after being heated, proceeds partial esterification reaction, while into polycondensation process.Room 2 under precondensation Precondensation under room vacuum orifice 2e be located at topmost, more higher toward upper strata vacuum, the vacuum in ceiling portion is 1 under precondensation ~10kpa(Absolute pressure), material progressively carries out polymerisation when through tower tray layer by layer, makes material in process from bottom to top The middle degree of polymerization is incrementally increased, and is finally discharged from precondensation discharging opening 2c.
The bottom centre for being esterified upper chamber 1 is provided with cyclone agitator disk 1h that is horizontally disposed and being centrosymmetric, cyclone agitator disk 1h is hollow cylinder plate, and the bottom centre of cyclone agitator disk 1h is connected with nitrogen inlet 1c, the circumferential wall of cyclone agitator disk 1h On be evenly distributed with multiple nitrogen jets mouthful 1h1, being respectively equipped with the outside of each nitrogen jet mouthful 1h1 makes what nitrogen was tangentially projected Nitrogen water conservancy diversion arc 1h2, 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, is sprayed from each nitrogen jet mouthful 1h1, warp The water conservancy diversion of nitrogen water conservancy diversion arc 1h2 is crossed, nitrogen is projected along the tangential direction of nitrogen water conservancy diversion arc tip circle everywhere, in esterification Level vortex is formed on the bottom of upper chamber 1, and fully material can be stirred, and nitrogen will also be moved to material upwards after projecting Form secondary agitation, it is ensured that material is thoroughly mixed uniformly.
Be esterified upper chamber 1 inner wall lower be provided with circumferentially and upper end open external flow guiding cylinder 1d, external flow guiding cylinder 1d with Esterification discharging annular groove 1e, external flow guiding cylinder 1d are formed between the esterification inwall of upper chamber 1 and is provided with external flow guiding cylinder material outlet 1d1 with esterification Discharging annular groove 1e is communicated, and esterification material outlet 1f is communicated 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 line coaxially therewith, the annular section between inner draft tube 1g and external flow guiding cylinder 1d is located at cyclone agitator disk 1h's Excircle top, the upper port of the upper port less than external flow guiding cylinder 1d of inner draft tube 1g;The inner chamber for being esterified upper chamber 1 is provided with along axis The center expects pipe in the middle part of inner draft tube 1g is extended downward, the upper end of center expects pipe is connected with material inlet 1a.
The nitrogen that cyclone agitator disk 1h is projected makes the material of esterification upper chamber bottom form strong circulation, in nitrogen and heating Under the thermal convection current double action of coil pipe, annulus of the material between inner draft tube 1g and external flow guiding cylinder 1d is moved upwards;It is interior Material inside guide shell 1g flows downward, and forms the state of inside and outside stream circulation, new material from the lower port of center expects pipe to After lower outflow, that is, it is involved in stream circulation and is stirred;At high temperature there is esterification in PTA powders with ethylene glycol, As new material constantly enters, the material for having reacted is esterified out from the external flow guiding cylinder material outlet 1d1 entrance of external flow guiding cylinder 1d Material annular groove 1e, continues to react thorough being esterified in heating jacket under the heating of heating agent during flowing, finally from esterification discharging ring The esterification material outlet 1f discharges of groove 1e bottoms.
Annulus is provided with multigroup esterification heating coil 1p, every group of heating medium for heating between external flow guiding cylinder 1d and inner draft tube 1g Coil pipe is respectively equipped with esterification heating coil Heating medium and the heating agent outlet of esterification heating coil.PTA powders are led outside with ethylene glycol While stir in annulus between flow cartridge 1d and inner draft tube 1g, while the heating of kettle heating coil is esterified, and can be with root Need to determine the group number of the esterifying kettle heating coil that input is heated according to technique.
External flow guiding cylinder material outlet 1d1 extends vertically downwards along the short transverse of external flow guiding cylinder 1d, esterification discharging annular groove 1e Inner chamber be provided with upper chamber radial direction diaphragm 1e1, external flow guiding cylinder material outlet 1d1 and be located at upper chamber respectively with esterification material outlet 1f The both sides of radial direction diaphragm 1e1;Room discharging annular groove 2b, room discharging ring under precondensation under precondensation are provided with above top tray The bottom of groove 2b is connected under precondensation on the barrel of room 2, and room discharging annular groove 2b is provided with vertically extending pre- under precondensation Room flash mouthful 2b1, precondensation discharging opening 2c are communicated with the bottom of discharging annular groove 2b in room under precondensation under polycondensation, and room goes out under precondensation The inner chamber of material annular groove 2b is provided with room radial direction diaphragm 2b2 under precondensation, room flash mouthful 2b1 and precondensation discharging opening under precondensation 2c is respectively positioned at the both sides of radial direction diaphragm 2b2 in room under precondensation.
Upper chamber radial direction diaphragm 1e1 separates material outlet 1f and external flow guiding cylinder material outlet 1d1 is esterified, and can prevent There is short stream in the material in esterification discharging annular groove 1e, material is had maximum stroke in esterification discharging annular groove 1e, and material enters Enter the form in laminar flow after esterification discharging annular groove 1e, along tower body inner wall surrounding one week, material continued by ester during advance Change heating jacket heating, finally from the 1f outflows of esterification material outlet, the structure extends material in esterification discharging annular groove 1e Heat time.Room radial direction diaphragm 2b2 separates room flash mouthful 2b1 and precondensation discharging opening 2c under precondensation under precondensation, Can prevent the material under precondensation in room discharging annular groove 2b from short stream occurring, material is had in room discharging annular groove 2b under the precondensation There is a stroke of maximum, material enters the form after room discharging annular groove 2b in laminar flow under precondensation, along tower body inner wall surrounding one week, Material continues to be heated by precondensation heating jacket during advance, is finally flowed out from precondensation discharging opening 2c, structure extension Heat time of the material under the precondensation in room discharging annular groove 2b.
Foam trapping disk 2d is provided with precondensation above room discharging annular groove 2b, foam trapping disk 2d is horizontally set on preshrunk The lower section of room vacuum orifice 2e on the cross section of poly- lower room 2 and under precondensation.A large amount of bubbles can be produced in polymerization process, is steeped Foam trapping disk 2d can prevent the bubble of room 2 under precondensation from entering under the precondensation of top room under room vacuum orifice 2e and precondensation Vacuum meter interface 2g.
Material the tedge 2a1, each material tedge 2a1 of multiple insertion tower trays are respectively uniformly distributed on each layer tower tray 2a Top be covered each by the material deflector cup 2a2 of line coaxially therewith, each material deflector cup 2a2 is that fornix shape and lower port are connected On tower tray 2a, deflector cup discharging opening 2a3 is uniformly provided with the lower circumference of each material deflector cup 2a2.Material rises from material The inner chamber of material deflector cup 2a2 is advanced on pipe 2a1, then baffling baffling downwards from material deflector cup 2a2 lower circumferences Cover discharging opening 2a3 flows out.Due to the polycondensation of the swabbing action and material of room vacuum orifice 2e under room top precondensation under precondensation Process, air cavity is formed at each layer of top of material deflector cup 2a2, and the vacuum in most last layer material deflector cup air cavity is most Height, more down the vacuum in material deflector cup air cavity progressively successively decrease, material from bottom to top passes sequentially through each layer tower tray and material Polymerisation is progressively carried out during deflector cup 2a2, material degree of polymerization during from bottom to top is incrementally increased.
The low head inner chamber for being esterified material preheater 3 is respectively equipped with horizontally disposed material distribution plate 3e, material distribution plate Multiple material dispensing orifice 3e1 are evenly distributed with 3e.Esterification material and auxiliary agent are distributed by numerous materials of material distribution plate 3e After the 3e1 of hole, can more uniformly into each heat exchanging pipe of top.
The barrel of esterification upper chamber 1 is provided with esterification upper chamber interface of the level gauge 1j and is communicated with the bottom of esterification discharging annular groove 1e, The aperture of esterification fluid level control valve V1 is controlled by the liquid level of esterification discharging annular groove 1e;The barrel of room 2 is provided with preshrunk under precondensation The discharge bottom of annular groove 2b of poly- lower room interface of the level gauge 2f and room under precondensation communicates, the aperture of precondensation fluid level control valve V2 or The flow rates controlled of precondensation melt conveying pump B1 is in the liquid level of discharging annular groove 2b in room under precondensation.
The bottom for being esterified heating jacket is provided with esterification upper chamber Heating medium 1m, is esterified the top of heating jacket and is provided with esterification Room heating agent outlet 1n;The bottom of precondensation heating jacket is provided with room Heating medium 2h under precondensation, precondensation heating jacket it is upper Portion is provided with heating agent outlet 2j in room under precondensation;The shell side bottom for being esterified material preheater 3 is provided with preheater Heating medium 3c, is esterified The shell side top of material preheater 3 is provided with preheater heating agent outlet 3d.
The job step of present invention esterification Prepolycondensating reactor is as follows successively:(1) after PTA powders and ethylene glycol mixing are beaten Enter the inner draft tube 1g of esterification upper chamber 1, each nitrogen jet mouthful 1h1 spray of the nitrogen from cyclone agitator disk 1h through center expects pipe Go out, forming level in the bottom of esterification upper chamber 1 by the water conservancy diversion of nitrogen water conservancy diversion arc 1h2 is vortexed, and nitrogen is moved to thing upwards Material forms secondary agitation, and material is under the thermal convection current double action of nitrogen and heating coil along inner draft tube 1g and external flow guiding cylinder 1d Between annulus move upwards, the material inside inner draft tube 1g flows downward, and forms inside and outside stream circulation.
(2) at high temperature there is esterification in PTA powders with ethylene glycol in esterification upper chamber 1, and the gauge pressure for being esterified upper chamber 1 is 0.5 ~2bar, the gaseous substance that esterification is produced is discharged from esterification upper chamber gaseous phase outlet 1b;As new material constantly enters, instead The material answered enters esterification discharging annular groove 1e from external flow guiding cylinder material outlet 1d1, is flowed one week in esterification discharging annular groove 1e And continuation is heated and makes reaction thoroughly, finally from the 1f discharges of esterification material outlet, by being esterified fluid level control valve V1 into esterification Thing discharge nozzle G1, the aperture of esterification fluid level control valve V1 is controlled by the liquid level of esterification discharging annular groove 1e, and auxiliary agent is from auxiliary agent import G1a It is added in carboxylate discharge nozzle G1.
(3) in the presence of potential difference and pressure difference, esterification material and auxiliary agent enter preheater and pass through material distribution plate 3e, help The gasification of excessive ethylene glycol produces bubble, the upward movement progress material of bubble simultaneously to stir in agent;Esterification material is upward after being heated Room 2 under into precondensation.
(4) material sequentially passes through each floor tower tray and proceeds partial esterification reaction upwards in room 2 under precondensation, 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, then rolls over Deflector cup discharging opening 2a3 outflows under flow direction from material deflector cup lower circumference, gas is formed at the top of material deflector cup 2a2 Chamber;Under precondensation the absolute pressure in ceiling portion be 1~10kpa, the vacuum highest in most last layer material deflector cup air cavity, more Down progressively successively decrease, material degree of polymerization during from bottom to top is incrementally increased, into precondensation under room discharging annular groove 2b, Flowed one week in room discharging annular groove 2b under precondensation and continue to be heated, finally discharged from precondensation discharging opening 2c, by preshrunk Poly- fluid level control valve V2 or precondensation melt conveying pump B1 enters precondensation discharge nozzle G2.The material esterification of precondensation discharging opening 2c Rate is more than 96%, and the degree of polymerization is more than 15.
The foregoing is only the preferable possible embodiments of the present invention, non-therefore limitation patent protection model of the invention Enclose.In addition to the implementation, the present invention can also have other embodiment, and such as heating agent can be conduction oil, or its Its heat carrier etc..The technical scheme that all use equivalents or equivalent transformation are formed, all falls within the protection domain of application claims It is interior.Technical characteristic of the present invention without description can be realized by or using prior art, will not be repeated here.

Claims (10)

1. the kettle system of a kind of fat polymerization two, including esterification Prepolycondensating reactor and without stirring polymer reactor, the esterification is pre- Polycondensation reactor is provided with material inlet and precondensation discharging opening, described to be provided with polymer reactor charging aperture without stirring polymer reactor With polymer discharge mouthful, the precondensation discharging opening is by precondensation fluid level control valve or precondensation melt conveying pump and precondensation Discharge nozzle is connected, and the precondensation discharge nozzle is connected with the polymer reactor charging aperture, it is characterised in that:It is described without stirring Polymer reactor includes the cylinder of vertical setting and closed at both ends, the top of cylinder lumen be provided with it is horizontal and by cylinder laterally every Disconnected cloth liquid disk, the cloth liquid disk is provided with up big and down small liquid distributing hole, film supplying tube is provided with the liquid distributing hole and both are coaxial Line, the film supplying tube extends straight down, and the inner chamber of the film supplying tube is plugged with polymer reactor heating medium for heating pipe, the cylinder External wall of upper portion be provided with polymer reactor vacuum orifice and the polymer reactor charging aperture, the lower end of the cylinder is provided with taper Head, the lower end of the conical head is provided with discharging spiral, and the polymer discharge mouthful is located at the lower end of the discharging spiral;The cylinder The periphery of body is provided with polymer reactor chuck, and the periphery of the conical head is provided with conical head chuck, the polymer reactor charging Mouth is located at the lower section of the cloth liquid disk, and the inwall of cylinder position corresponding with the polymer reactor charging aperture is provided with ring-type Cloth liquid bath, leave uniform annular slot between the lower end of the cloth liquid bath and cylinder inboard wall;The lower inner wall of the cylinder It is provided with the collecting tank of ring-type, the upper end open and lower end closed of the collecting tank;The outer wall of the cylinder is provided with and the collection The middle melt outlet that the bottom of liquid bath communicates, the middle melt outlet is connected with the entrance of middle melt conveying pump, described The outlet of middle melt conveying pump is connected with middle melt inlet, and the middle melt inlet is located on cylinder body outer wall and positioned at institute State the top of cloth liquid disk.
2. the kettle system of fat polymerization according to claim 1 two, it is characterised in that:Falling liquid film is provided with above the cloth liquid disk Pipe dividing plate, is provided with polymer reactor heating medium for heating pipe dividing plate above the film supplying tube dividing plate, the film supplying tube dividing plate and described Polymer reactor heating medium for heating pipe dividing plate respectively by cylinder laterally separate, the polymer reactor heating medium for heating pipe dividing plate it is upper Side is provided with polymer reactor upper cover;The upper port of the film supplying tube is connected on the pore of the film supplying tube dividing plate, described poly- The upper port for closing reactor heating medium for heating pipe is connected on the pore of the polymer reactor heating medium for heating pipe dividing plate;The polymerization Be connected with film supplying tube Heating medium on reactor upper cover, the film supplying tube dividing plate and polymer reactor heating medium for heating pipe dividing plate it Between barrel wall on be connected with film supplying tube heating agent outlet.
3. the kettle system of fat polymerization according to claim 1 two, it is characterised in that:The cylinder inboard wall is provided with downward spiral The barrel material distribution ring of extension, the upper end of the barrel material distribution ring is located at the outlet lower section of the cloth liquid bath, the cylinder The lower end of wall material distribution ring be located at the collecting tank upper port top, the barrel material distribution ring be semi-circular cross-section and Plane is connected on the cylinder inboard wall.
4. the kettle system of fat polymerization according to claim 1 two, it is characterised in that:Outside film supplying tube below the liquid distributing hole Wall is uniformly provided with least one film supplying tube material distribution ring, and the section of the film supplying tube material distribution ring is small broad in the middle in two Cydariform.
5. the kettle system of fat polymerization according to claim 1 two, it is characterised in that:The esterification Prepolycondensating reactor includes It is separated into by arc-shaped partition in the vertical tower body of closing, the vertical column body and is esterified room under upper chamber and precondensation, in the esterification The barrel of room is externally provided with esterification heating jacket, and the barrel of room is externally provided with precondensation heating jacket under the precondensation;The esterification Esterification upper chamber gaseous phase outlet and the material inlet are provided with the top of upper chamber, the bottom centre of the arc-shaped partition is provided with nitrogen and enters Mouthful, the side wall of the esterification upper chamber is provided with esterification material outlet;The bottom of room is connected with esterification material preheating under the precondensation Device, the low head bottom of the esterification material preheater is provided with preheater charging aperture, and the esterification material outlet passes through esterifying liquid Level control valve and carboxylate discharge nozzle are connected with the preheater charging aperture, and being connected with auxiliary agent on the carboxylate discharge nozzle enters Mouthful, the preheater discharging opening of the esterification material preheater upper end is connected with the bottom inlet of room under the precondensation;It is described pre- The inner chamber of room is provided with multilayer tower tray from bottom to top under polycondensation, and the precondensation discharging opening is located at the top cylinder of room under the precondensation On wall, room vacuum orifice under precondensation is provided with above the precondensation discharging opening.
6. the kettle system of fat polymerization according to claim 5 two, it is characterised in that:The bottom centre of the esterification upper chamber sets There is cyclone agitator disk that is horizontally disposed and being centrosymmetric, the cyclone agitator disk is hollow cylinder plate, the cyclone stirring The bottom centre of disk is connected with the nitrogen inlet, and multiple nitrogen jets are evenly distributed with the circumferential wall of the cyclone agitator disk Mouthful, the outside of each nitrogen jet mouthful is respectively equipped with the nitrogen water conservancy diversion arc for making nitrogen tangentially project, each nitrogen The root of water conservancy diversion arc is connected in the circumferential wall of the cyclone agitator disk.
7. the kettle system of fat polymerization according to claim 6 two, it is characterised in that:The inner wall lower of the esterification upper chamber sets Have circumferentially and upper end open external flow guiding cylinder, esterification discharging ring is formed between the external flow guiding cylinder and the upper chamber interior walls of esterification Groove, the external flow guiding cylinder is provided with external flow guiding cylinder material outlet and is communicated with the esterification discharging annular groove, the esterification material outlet Bottom with the esterification discharging annular groove communicates;The inner chamber of the external flow guiding cylinder is provided with the inner draft tube of line coaxially therewith, described Annular section between inner draft tube and the external flow guiding cylinder is located at the excircle top of the cyclone agitator disk, the Inner guide Upper port of the upper port of cylinder less than external flow guiding cylinder;The inner chamber of the esterification upper chamber is provided with and extends downward inner draft tube along axis The center expects pipe at middle part, the upper end of the center expects pipe is connected with the material inlet;The external flow guiding cylinder and inner draft tube it Between annulus be provided with multigroup esterification heating coil, every group of heating medium for heating coil pipe be respectively equipped with esterification heating coil Heating medium and The heating agent outlet of esterification heating coil.
8. the kettle system of fat polymerization according to claim 7 two, it is characterised in that:The external flow guiding cylinder material outlet is along institute The short transverse for stating external flow guiding cylinder extends vertically downwards, and the inner chamber of the esterification discharging annular groove is provided with upper chamber radial direction diaphragm, The external flow guiding cylinder material outlet is with the esterification material outlet respectively positioned at the both sides of the upper chamber radial direction diaphragm;Top layer Discharging annular groove in room under precondensation is provided with above tower tray, the bottom of room discharging annular groove is connected to the precondensation under the precondensation On the barrel of lower room, room discharging annular groove is provided with room flash mouthful under vertically extending precondensation under the precondensation, described pre- Polycondensation discharging opening is communicated with the bottom of discharging annular groove in room under the precondensation, and the inner chamber of room discharging annular groove is provided with the precondensation Radial direction diaphragm in room under precondensation, room flash mouthful is located at the preshrunk respectively with the precondensation discharging opening under the precondensation The both sides of poly- lower room radial direction diaphragm.
9. the kettle system of fat polymerization according to claim 5 two, it is characterised in that:Uniform point respectively on each layer tower tray The material tedge of multiple insertion tower trays is furnished with, the material of line coaxially therewith is covered each by above each material tedge Deflector cup, each material deflector cup is that fornix shape and lower port are connected on the tower tray, under each material deflector cup Deflector cup discharging opening is uniformly provided with portion's circumference.
10. the kettle system of fat polymerization according to claim 8 two, it is characterised in that:Discharging annular groove in room under the precondensation Top be provided with foam trapping disk, foam trapping disk is horizontally set under the precondensation on the cross section of room and positioned at institute State the lower section of room vacuum orifice under precondensation;The low head inner chamber of the esterification material preheater is respectively equipped with horizontally disposed thing Material distribution plate, is evenly distributed with multiple material dispensing orifices on the material distribution plate.
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