CN105664796A - Vertical esterification pre-polycondensation reactor and esterification pre-polycondensation reaction method - Google Patents
Vertical esterification pre-polycondensation reactor and esterification pre-polycondensation reaction method Download PDFInfo
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- CN105664796A CN105664796A CN201610097835.2A CN201610097835A CN105664796A CN 105664796 A CN105664796 A CN 105664796A CN 201610097835 A CN201610097835 A CN 201610097835A CN 105664796 A CN105664796 A CN 105664796A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
- B01J3/048—Multiwall, strip or filament wound vessels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/14—Production of inert gas mixtures; Use of inert gases in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/185—Details relating to the spatial orientation of the reactor vertical
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/24—Stationary reactors without moving elements inside
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Abstract
The invention relates to a vertical esterification pre-polycondensation reactor and an esterification pre-polycondensation reaction method. A tower body is divided into an upper esterification chamber and a lower esterification chamber by an arc-shaped partition plate, wherein a material inlet and a gas phase outlet are formed in the top of the upper esterification chamber, a nitrogen inlet is formed in the bottom, and an esterification material outlet is formed in the side wall. The bottom of a lower pre-polycondensation chamber is connected with a pre-heater, the esterification material outlet is connected with a feeding port of the pre-heater, and a discharging port of the pre-heater is connected with the bottom of the lower pre-polycondensation chamber. Multiple layers of trays are arranged in the inner cavity of the lower pre-polycondensation chamber, and a polymer discharging port and a vacuum orifice are formed in the upper-wall cylindrical wall of the lower pre-polycondensation chamber. A material is firstly fed into the upper esterification chamber for esterification reaction, the esterification product is fed into the pre-heater under the effects of differential pressure and potential difference, is pre-heated and then is fed into the lower pre-polycondensation chamber for polycondensation, the polymerization degree of the material is gradually increased in the lower pre-polycondensation chamber from bottom to top, and the material is finally discharged from the polymer discharging port. The esterification chambers and the pre-polycondensation chambers are connected integrally, so that the vertical esterification pre-polycondensation reactor is compact in structure, small in heat loss and high in production efficiency.
Description
Technical field
The present invention relates to a kind of vertical esterification Prepolycondensating reactor, the invention still further relates to a kind of method being esterified prepolymerization reaction, belong to polyester producing process field.
Background technology
In prior art, esterification and polycondensation reaction during production of polyester are typically in separate reaction tower or reactor to carry out, if publication number is the Chinese invention patent of CN101618304B, disclose a kind of esterifier, it is made up of polylith column plate, all installing a downspout and a riser on every block of column plate, riser connects rotatable gas distributor, and 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, has solid catalyst in liquid. Liquid phase is the component containing carboxylic acid, in the reactor downwards by one block of esterification column plate current to next block column plate, react with the alcohol steam counter-flow risen.
Publication number is the Chinese utility model patent of CN2741645, disclose a kind of polycondensation reaction tower in polycondensation reaction device field, including the double Shell being made up of inner housing and shell body, it it is chuck between inner housing and shell body, the heating agent being communicated with chuck on shell body enters, outlet, double Shell is communicated with the steam outlet port of 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 it are provided with between charging aperture and discharging opening, described tower tray includes housing, some material leakage passages it are 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 big, and production efficiency is low.
Summary of the invention
The primary and foremost purpose of the present invention is in that, overcomes problems of the prior art, it is provided that a kind of vertical esterification Prepolycondensating reactor, compact conformation, and floor space is little, and production efficiency is high.
For solving above technical problem, the vertical esterification Prepolycondensating reactor of one of the present invention, including the vertical tower body closed, it is separated into room under the upper room of esterification and precondensation by arc-shaped partition in described vertical column body, in described esterification, the barrel of room is externally provided with esterification heating jacket, and under described precondensation, the barrel of room is externally provided with precondensation heating jacket;In described esterification, the top of room is provided with material inlet and esterification upper room gaseous phase outlet, 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 to esterification material preheater, it is provided with preheater charging aperture 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, being connected to auxiliary agent import on described carboxylate discharge nozzle, 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 multilamellar tower tray from bottom to top, under described precondensation, the top barrel of room is provided with polymer discharge mouth, described polymer discharge mouth is connected with polymer discharge pipe by precondensation fluid level control valve, described polymer discharge mouth be arranged over vacuum orifice.
Relative to prior art, the present invention achieves following beneficial effect: PTA powder and ethylene glycol mixing enter room esterification from material inlet after pulling an oar, nitrogen enters room esterification from the nitrogen inlet bottom arc-shaped partition, it is stirred material making its mix homogeneously, in esterification under the hot environment of room, 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, simultaneously works as stirring action, it is upwardly under precondensation after esterification material is heated room, proceeds partial esterification reaction, simultaneously enter polycondensation process, under precondensation, the vacuum orifice of room is positioned at topmost, more more high toward upper strata vacuum, under precondensation, the vacuum in ceiling portion is 1～10kpa(absolute pressure), material progressively carries out polyreaction when through tower tray layer by layer, make material degree of polymerization in process from bottom to top incrementally increase, finally discharge from polymer discharge mouth. 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, it is not necessary to extra power material can flow to room under precondensation, mechanical agitating device 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 the cyclone agitator disk being horizontally disposed with and being 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 making nitrogen tangentially penetrate, 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, water conservancy diversion through 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, fully material can be stirred, also to move upward after nitrogen injection and material is formed secondary stirring, it is ensured that material is thoroughly mixed uniformly.
Improvement as 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, esterification discharging annular groove is formed between described external flow guiding cylinder and the upper chamber interior walls of esterification, 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 line coaxially therewith, 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 extends downward the center material pipe in the middle part of inner draft tube along axis, and the upper end of described center material pipe is connected with described material inlet. The nitrogen of cyclone agitator disk injection makes in esterification the material bottom room form strong circulation, and under the thermal convection current dual function of nitrogen and heating coil, material moves upward along the annulus between inner draft tube and external flow guiding cylinder; Material within inner draft tube flows downward, and forms the state of inside and outside stream circulation, from center, new material expects that the lower port of pipe flows downward out after, is namely involved in stream circulation and is stirred; 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, esterification heating jacket continues reaction thoroughly in flow process under the heating of heating agent, finally discharges from the esterification material outlet bottom esterification discharging annular groove.
As a further improvement on the present invention, between described external flow guiding cylinder and inner draft tube, annulus is provided with many group esterification heating coils, and often group heating medium for heating coil pipe is respectively equipped with esterification heating coil Heating medium and esterification heating coil heating agent outlet. PTA powder and ethylene glycol between external flow guiding cylinder and inner draft tube in annulus while stirring, esterified still heating coil heats, and can need to determine to put into the group number of esterifying kettle heating coil that heat according to technique.
As a further improvement on the present invention, described external flow guiding cylinder material outlet extends vertically downwards along the short transverse of described external flow guiding cylinder, the inner chamber room of being provided with of described esterification discharging annular groove is diaphragm radially, and described external flow guiding cylinder material outlet and described esterification material outlet lay respectively at the both sides of described upper room radially diaphragm; Top tray be arranged over polymer discharge annular groove, the bottom of described polymer discharge annular groove is connected under described precondensation on the barrel of room, described polymer discharge annular groove is provided with vertically extending polymer flash mouth, described polymer discharge mouth communicates with the bottom of described polymer discharge annular groove, the inner chamber of described polymer discharge annular groove is provided with lower room radially diaphragm, and described polymer flash mouth and described polymer discharge mouth lay respectively at the both sides of described lower room radially diaphragm. Esterification material outlet and external flow guiding cylinder material outlet are separated by upper room radially diaphragm, there is short stream in the material being possible to prevent in esterification discharging annular groove, 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, round along cylinder inboard wall, material continue in advance process esterified heating jacket heating, finally from esterification material outlet flow out, this structure extend material esterification discharging annular groove in heat time heating time. Polymer flash mouth and polymer discharge mouth are separated by lower room radially diaphragm, it is possible to prevent the material in polymer discharge annular groove that short stream occurs, material is made to have maximum stroke in polymer discharge annular groove, material is the form of laminar flow after entering polymer discharge annular groove, round along cylinder inboard wall, material continues to be heated by precondensation heating jacket in advance process, finally flows out from polymer discharge mouth, and this structure extends material heat time heating time in polymer discharge annular groove.
As a further improvement on the present invention, described polymer discharge annular groove be arranged over foam trapping dish, described foam trapping dish is horizontally set under described precondensation on the cross section of room and is positioned at the lower section of described vacuum orifice. Producing a large amount of bubble in polymerization process, foam trapping dish can stop the bubble of room under precondensation to enter vacuum orifice and the vacuum meter interface of top.
As a further improvement on the present invention, the described tower tray of each layer is respectively uniformly distributed the material tedge of multiple through tower tray, the top of each described material tedge is covered each by the material deflector cup of line coaxially therewith, 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 uniformly 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 polycondensation process of the swabbing action of top, room vacuum orifice and material under precondensation, air cavity is formed at the top of each layer of material deflector cup, vacuum in most last layer material deflector cup air cavity is the highest, more down the vacuum in material deflector cup air cavity is progressively successively decreased, material from bottom to top passes sequentially through in the process of each layer tower tray and material deflector cup and progressively carries out polyreaction, and material degree of polymerization in process from bottom to top incrementally increases.
As a further improvement on the present invention, 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. Esterification material and auxiliary agent are after numerous material dispensing orifices of material distribution plate, it is possible to more uniformly enter each heat exchanging pipe of top.
As a further improvement on the present invention, in described esterification, the barrel of room is provided with room interface of the level gauge and communicates with the bottom of described esterification discharging annular groove, and the aperture of described esterifying liquid level control valve is controlled by the liquid level of described esterification discharging annular groove; Under described precondensation, the barrel of room is provided with lower room interface of the level gauge and communicates with the bottom of described polymer discharge annular groove, and the aperture of described precondensation fluid level control valve is controlled by the liquid level of described polymer discharge annular groove; The bottom of described esterification heating jacket is provided with room Heating medium, and the top of described esterification heating jacket is provided with room heating agent outlet; The bottom of described precondensation heating jacket is provided with lower room Heating medium, and the top of described precondensation heating jacket is provided with the heating agent outlet of lower room; The shell side bottom of described esterification material preheater is provided with preheater Heating medium, and the shell side top of described esterification material preheater is provided with the outlet of preheater heating agent; In described esterification, the top of room is provided with pressure gauge connection, and under described precondensation, the top of room is provided with vacuum meter interface.
Further object is that, overcome problems of the prior art, it is provided that a kind of method being esterified prepolymerization reaction, floor space is little, and heat loss is few, and production efficiency is high.
For solving above technical problem, the present invention is esterified the method for prepolymerization reaction, in turn include the following steps: (1) PTA powder and ethylene glycol mixing making beating Hou Jing center material pipe enter the inner draft tube of the upper room of esterification, nitrogen sprays from each nitrogen jet mouth of cyclone agitator disk, horizontal vortex is formed through water conservancy diversion bottom of room in esterification of nitrogen water conservancy diversion arc, nitrogen moves upward and material is formed secondary stirring, material moves upward along the annulus between inner draft tube and external flow guiding cylinder under the thermal convection current dual function of nitrogen and heating coil, material within inner draft tube flows downward, form inside and outside stream circulation,(2) at high temperature there is esterification in PTA powder and ethylene glycol room in esterification, and in esterification, the gauge pressure of room is 0.5～2bar, and the gaseous substance that esterification produces is discharged from room gaseous phase outlet esterification; Along with new material constantly enters, the material reacted enters esterification discharging annular groove from external flow guiding cylinder material outlet, in esterification discharging annular groove, flowing one week continuation are heated and make reaction thorough, last from esterification material outlet discharge, carboxylate discharge nozzle is entered by esterifying liquid level control valve, the aperture of esterifying liquid level control valve is controlled by the liquid level of esterification discharging annular groove, and auxiliary agent is added in carboxylate discharge nozzle; (3) under the effect of potential difference and pressure reduction, being esterified material and auxiliary agent enters preheater and through material distribution plate, ethylene glycol gasification excessive in auxiliary agent produces bubble, and bubble moves upward and promotes material and stir; It is upwardly under precondensation after esterification material is heated room; (4) under precondensation, in room, material upwards sequentially passes through each floor tower tray and proceeds partial esterification reaction, and enters polycondensation process; When through tower tray, 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, forms air cavity at the top of material deflector cup; Under precondensation, the absolute pressure in ceiling portion is 1～10kpa, vacuum in most last layer material deflector cup air cavity is the highest, more down progressively successively decrease, material degree of polymerization in process from bottom to top incrementally increases, enter polymer discharge annular groove, polymer discharge annular groove flow one week and continues heated, finally discharging from polymer discharge mouth, enter polymer discharge pipe by precondensation fluid level control valve.
Relative to prior art, the present invention achieves following beneficial effect: esterification room and precondensation room are connected as a single entity by the present invention, compact conformation, floor space is little, and heat loss is few, it is not necessary to extra power material can flow to room under precondensation from room esterification, mechanical agitating device, save energy consumption, reduced fault rate, improve production efficiency.
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 use is described, is not used to the restriction present invention.
Fig. 1 is the structural representation of the vertical esterification Prepolycondensating reactor of the present invention.
Fig. 2 is the flow direction of material figure of esterification discharging annular groove.
Fig. 3 is the sectional view of cyclone agitator disk.
Fig. 4 is the structural representation of material distribution plate.
Fig. 5 is the enlarged drawing of aminoacyl site in Fig. 1.
Fig. 6 is the flow direction of material figure of polymer discharge annular groove.
In figure: 1. the upper room of 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. is esterified discharging annular groove; The upper room of 1e1. radially diaphragm; 1f. is esterified material outlet; 1g. inner draft tube; 1h. cyclone agitator disk; 1h1. nitrogen jet mouth; 1h2. nitrogen water conservancy diversion arc; 1j. upper room interface of the level gauge; 1k. pressure gauge connection; 1m. upper room Heating medium; The heating agent outlet of 1n. upper room; 1p. is esterified heating coil;
2. room under precondensation; 2a. tower tray; 2a1. material tedge; 2a2. material deflector cup; 2a3. deflector cup discharging opening; 2b. polymer discharge annular groove; 2b1. polymer flash mouth; Room radially diaphragm under 2b2.; 2c. polymer discharge mouth; 2d. foam trapping dish; 2e. vacuum orifice; Room interface of the level gauge under 2f.;2g. vacuum meter interface; Room Heating medium under 2h.; Heating agent outlet in room under 2j.;
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;
G1. carboxylate discharge nozzle; G1a. auxiliary agent import; G2. polymer discharge pipe; V1. esterifying liquid level control valve; V2. precondensation fluid level control valve.
Detailed description of the invention
As shown in Figures 1 to 6, the vertical esterification Prepolycondensating reactor of the present invention includes the vertical tower body closed, it is separated into room 2 under the upper room 1 of esterification and precondensation by arc-shaped partition in vertical column body, in esterification, the barrel of room 1 is externally provided with esterification heating jacket, and under precondensation, the barrel of room 2 is externally provided with precondensation heating jacket; In esterification, the top of room 1 is provided with material inlet 1a and the upper room gaseous phase outlet 1b of 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 pressure gauge connection 1k.
Under precondensation, the bottom of room 2 is connected to esterification material preheater 3, it is provided with preheater charging aperture 3a bottom the low head of esterification material preheater 3, esterification material outlet 1f is connected with preheater charging aperture 3a with carboxylate discharge nozzle G1 by esterifying liquid level control valve V1, being connected to auxiliary agent import G1a on carboxylate discharge nozzle G1, 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 multilamellar tower tray 2a from bottom to top, under precondensation, the top barrel of room 2 is provided with polymer discharge mouth 2c, polymer discharge mouth 2c is connected with polymer discharge pipe G2 by precondensation fluid level control valve V2, and polymer discharge mouth 2c is arranged over vacuum orifice 2e and vacuum meter interface 2g.
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, it is stirred material making its mix homogeneously, in esterification under the hot environment of room 1, 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 room gaseous phase outlet 1b 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, simultaneously works as stirring action. it is upwardly under precondensation after esterification material is heated room 2, proceeds partial esterification reaction, simultaneously enter polycondensation process. under precondensation, the vacuum orifice 2e of room 2 is positioned at topmost, more more high toward upper strata vacuum, under precondensation, the vacuum in ceiling portion is 1～10kpa(absolute pressure), material progressively carries out polyreaction when through tower tray layer by layer, make material degree of polymerization in process from bottom to top incrementally increase, finally discharge from polymer discharge mouth 2c.
In esterification, the bottom centre of room 1 is provided with the cyclone agitator disk 1h being horizontally disposed with and being 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 making nitrogen tangentially penetrate, 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, water conservancy diversion through 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, fully material can be stirred, also to move upward after nitrogen injection and material is formed secondary stirring, it is ensured that material is thoroughly mixed uniformly.
In esterification, the inner wall lower of room 1 is provided with circumferentially and the external flow guiding cylinder 1d of upper end open, esterification discharging annular groove 1e is formed between external flow guiding cylinder 1d and esterification upper room 1 inwall, external flow guiding cylinder 1d is provided with external flow guiding cylinder material outlet 1d1 and communicates with esterification discharging annular groove 1e, and the bottom of esterification material outlet 1f and esterification discharging annular groove 1e communicates; The inner chamber of external flow guiding cylinder 1d is provided with the inner draft tube 1g of line coaxially therewith, 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, the upper port of the inner draft tube 1g upper port lower than external flow guiding cylinder 1d; In esterification, the inner chamber of room 1 is provided with and extends downward the center material pipe in the middle part of inner draft tube 1g along axis, and the upper end of center material pipe is connected with material inlet 1a.
The nitrogen of cyclone agitator disk 1h injection makes in esterification the material bottom room form strong circulation, and under the thermal convection current dual function of nitrogen and heating coil, material moves upward along the annulus between inner draft tube 1g and external flow guiding cylinder 1d; Material within inner draft tube 1g flows downward, and forms the state of inside and outside stream circulation, from center, new material expects that the lower port of pipe flows downward out after, is namely involved in stream circulation and is stirred; 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, esterification heating jacket continues reaction thoroughly in flow process under the heating of heating agent, finally discharges 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 many group esterification heating coil 1p, and often group heating medium for heating coil pipe is respectively equipped with esterification heating coil Heating medium and esterification heating coil heating agent outlet. PTA powder and ethylene glycol between external flow guiding cylinder 1d and inner draft tube 1g in annulus while stirring, esterified still heating coil heats, and can need to determine to put into the group number of esterifying kettle heating coil that heat according to technique.
External flow guiding cylinder material outlet 1d1 extends vertically downwards along the short transverse of external flow guiding cylinder 1d, the inner chamber room of being provided with of esterification discharging annular groove 1e radially diaphragm 1e1, external flow guiding cylinder material outlet 1d1 and the both sides being esterified the material outlet 1f room of laying respectively at radially diaphragm 1e1; Top tray be arranged over polymer discharge annular groove 2b, on the barrel that the bottom of polymer discharge annular groove 2b is connected under precondensation room 2, polymer discharge annular groove 2b is provided with vertically extending polymer flash mouth 2b1, the bottom of polymer discharge mouth 2c and polymer discharge annular groove 2b communicates, the inner chamber of polymer discharge annular groove 2b is provided with lower room radially diaphragm 2b2, polymer flash mouth 2b1 and polymer discharge mouth 2c and lays respectively at the both sides of lower room radially diaphragm 2b2.
Esterification material outlet 1f and external flow guiding cylinder material outlet 1d1 is separated by upper room radially diaphragm 1e1, there is short stream in the material being possible to prevent in esterification discharging annular groove 1e, 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, round along cylinder inboard wall, material continues the heating of esterified heating jacket in advance process, last flowing out from esterification material outlet 1f, this structure extends material heat time heating time in esterification discharging annular groove 1e.Polymer flash mouth 2b1 and polymer discharge mouth 2c is separated by lower room radially diaphragm 2b2, it is possible to prevent the material in polymer discharge annular groove 2b that short stream occurs, material is made to have maximum stroke in polymer discharge annular groove 2b, material is the form of laminar flow after entering polymer discharge annular groove 2b, round along cylinder inboard wall, material continues to be heated by precondensation heating jacket in advance process, last flowing out from polymer discharge mouth 2c, this structure extends material heat time heating time in polymer discharge annular groove 2b.
The lower section being arranged on the cross section that foam trapping dish 2d, foam trapping dish 2d are horizontally set under precondensation room 2 and being positioned at vacuum orifice 2e of polymer discharge annular groove 2b. Producing a large amount of bubble in polymerization process, foam trapping dish 2d can stop the bubble of room 2 under precondensation to enter the vacuum orifice 2e and vacuum meter interface 2g of top.
Each layer tower tray 2a is respectively uniformly distributed the material tedge 2a1 of multiple through tower tray, the top of each material tedge 2a1 is covered each by the material deflector cup 2a2 of line coaxially therewith, 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 uniformly 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 polycondensation process of the swabbing action of top, room vacuum orifice 2e and material under precondensation, air cavity is formed at the top of each layer of material deflector cup 2a2, vacuum in most last layer material deflector cup air cavity is the highest, more down the vacuum in material deflector cup air cavity is progressively successively decreased, material from bottom to top passes sequentially through in the process of each layer tower tray and material deflector cup 2a2 and progressively carries out polyreaction, and material degree of polymerization in process from bottom to top incrementally increases.
The low head inner chamber of esterification material preheater 3 is respectively equipped with horizontally disposed material distribution plate 3e, and material distribution plate 3e is evenly distributed with multiple material dispensing orifice 3e1. Esterification material and auxiliary agent are after numerous material dispensing orifice 3e1 of material distribution plate 3e, it is possible to more uniformly enter each heat exchanging pipe of top.
In esterification the barrel of room 1 be provided with room interface of the level gauge 1j and esterification discharging annular groove 1e bottom communicate, the aperture of esterifying liquid level control valve V1 be controlled by esterification discharging annular groove 1e liquid level; Under precondensation, the barrel of room 2 is provided with the bottom of lower room interface of the level gauge 2f and polymer discharge annular groove 2b and communicates, and the aperture of precondensation fluid level control valve V2 is controlled by the liquid level of polymer discharge annular groove 2b.
The bottom of esterification heating jacket is provided with room Heating medium 1m, and the top of esterification heating jacket is provided with room heating agent outlet 1n; The bottom of precondensation heating jacket is provided with lower room Heating medium 2h, and the top of precondensation heating jacket is provided with lower room heating agent outlet 2j; 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 present invention is esterified the method for prepolymerization reaction, in turn include the following steps: (1) PTA powder and ethylene glycol mixing making beating Hou Jing center material pipe enter the inner draft tube 1g of the upper room 1 of esterification, nitrogen sprays from each nitrogen jet mouth 1h1 of cyclone agitator disk 1h, horizontal vortex is formed through water conservancy diversion bottom of room 1 in esterification of nitrogen water conservancy diversion arc 1h2, nitrogen moves upward and material is formed secondary stirring, material moves upward along the annulus between inner draft tube 1g and external flow guiding cylinder 1d under the thermal convection current dual function of nitrogen and heating coil, material within inner draft tube 1g flows downward, form inside and outside stream circulation.
(2) at high temperature room 1 there is esterification with ethylene glycol in PTA powder 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 room gaseous phase outlet 1b esterification; Along with new material constantly enters, the material reacted enters esterification discharging annular groove 1e from external flow guiding cylinder material outlet 1d1, in esterification discharging annular groove 1e, flowing one week continuation are heated and make reaction thorough, last from esterification material outlet 1f discharge, 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, being esterified material and auxiliary agent enters 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; It is upwardly under precondensation after esterification material is heated room 2.
(4) under precondensation, in room 2, material upwards sequentially passes through each floor tower tray and proceeds partial esterification reaction, 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 in ceiling portion is 1～10kpa, vacuum in most last layer material deflector cup air cavity is the highest, more down progressively successively decrease, material degree of polymerization in process from bottom to top incrementally increases, enter polymer discharge annular groove 2b, polymer discharge annular groove 2b flow one week and continues heated, finally discharging from polymer discharge mouth 2c, enter polymer discharge pipe G2 by precondensation fluid level control valve V2.
The foregoing is only the preferably possible embodiments of the present invention, the non-scope of patent protection therefore limiting to the present invention. In addition to the implementation, the present invention can also have other embodiments. All employings are equal to replacement or the technical scheme of equivalent transformation formation, all fall within 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 vertical esterification Prepolycondensating reactor, including the vertical tower body closed, it is characterized in that: in described vertical column body, be separated into room under the upper room of esterification and precondensation by arc-shaped partition, in described esterification, the barrel of room is externally provided with esterification heating jacket, and under described precondensation, the barrel of room is externally provided with precondensation heating jacket; In described esterification, the top of room is provided with material inlet and esterification upper room gaseous phase outlet, 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 to esterification material preheater, it is provided with preheater charging aperture 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, being connected to auxiliary agent import on described carboxylate discharge nozzle, 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 multilamellar tower tray from bottom to top, under described precondensation, the top barrel of room is provided with polymer discharge mouth, described polymer discharge mouth is connected with polymer discharge pipe by precondensation fluid level control valve, described polymer discharge mouth be arranged over vacuum orifice.
2. vertical esterification Prepolycondensating reactor according to claim 1, it is characterized in that: in described esterification, the bottom centre of room is provided with the cyclone agitator disk being horizontally disposed with and being 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 making nitrogen tangentially penetrate, the root of each described nitrogen water conservancy diversion arc is connected in the circumferential wall of described cyclone agitator disk.
3. vertical esterification Prepolycondensating reactor according to claim 2, 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, esterification discharging annular groove is formed between described external flow guiding cylinder and the upper chamber interior walls of esterification, 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 line coaxially therewith, 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 extends downward the center material pipe in the middle part of inner draft tube along axis, and the upper end of described center material pipe is connected with described material inlet.
4. vertical esterification Prepolycondensating reactor according to claim 3, it is characterized in that: between described external flow guiding cylinder and inner draft tube, annulus is provided with many group esterification heating coils, often group heating medium for heating coil pipe is respectively equipped with esterification heating coil Heating medium and esterification heating coil heating agent outlet.
5. vertical esterification Prepolycondensating reactor according to claim 3, it is characterized in that: described external flow guiding cylinder material outlet extends vertically downwards along the short transverse of described external flow guiding cylinder, the inner chamber room of being provided with of described esterification discharging annular groove is diaphragm radially, and described external flow guiding cylinder material outlet and described esterification material outlet lay respectively at the both sides of described upper room radially diaphragm; Top tray be arranged over polymer discharge annular groove, the bottom of described polymer discharge annular groove is connected under described precondensation on the barrel of room, described polymer discharge annular groove is provided with vertically extending polymer flash mouth, described polymer discharge mouth communicates with the bottom of described polymer discharge annular groove, the inner chamber of described polymer discharge annular groove is provided with lower room radially diaphragm, and described polymer flash mouth and described polymer discharge mouth lay respectively at the both sides of described lower room radially diaphragm.
6. vertical esterification Prepolycondensating reactor according to claim 5, it is characterized in that: described polymer discharge annular groove be arranged over foam trapping dish, described foam trapping dish is horizontally set under described precondensation on the cross section of room and is positioned at the lower section of described vacuum orifice.
7. vertical esterification Prepolycondensating reactor according to claim 1, it is characterized in that: the described tower tray of each layer is respectively uniformly distributed the material tedge of multiple through tower tray, the top of each described material tedge is covered each by the material deflector cup of line coaxially therewith, 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 uniformly provided with deflector cup discharging opening.
8. vertical esterification Prepolycondensating reactor according to claim 1, it is characterised in that: 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.
9. vertical esterification Prepolycondensating reactor according to claim 1, it is characterized in that: in described esterification, the barrel of room is provided with room interface of the level gauge and communicates with the bottom of described esterification discharging annular groove, and the aperture of described esterifying liquid level control valve is controlled by the liquid level of described esterification discharging annular groove; Under described precondensation, the barrel of room is provided with lower room interface of the level gauge and communicates with the bottom of described polymer discharge annular groove, and the aperture of described precondensation fluid level control valve is controlled by the liquid level of described polymer discharge annular groove; The bottom of described esterification heating jacket is provided with room Heating medium, and the top of described esterification heating jacket is provided with room heating agent outlet; The bottom of described precondensation heating jacket is provided with lower room Heating medium, and the top of described precondensation heating jacket is provided with the heating agent outlet of lower room; The shell side bottom of described esterification material preheater is provided with preheater Heating medium, and the shell side top of described esterification material preheater is provided with the outlet of preheater heating agent; In described esterification, the top of room is provided with pressure gauge connection, and under described precondensation, the top of room is provided with vacuum meter interface.
10. the method that the vertical esterification Prepolycondensating reactor adopted according to any one of claim 5 to 9 carries out esterification prepolymerization reaction, it is characterized in that, in turn include the following steps: (1) PTA powder and ethylene glycol mixing making beating Hou Jing center material pipe enter the inner draft tube of the upper room of esterification, nitrogen sprays from each nitrogen jet mouth of cyclone agitator disk, horizontal vortex is formed through water conservancy diversion bottom of room in esterification of nitrogen water conservancy diversion arc, nitrogen moves upward and material is formed secondary stirring, material moves upward along the annulus between inner draft tube and external flow guiding cylinder under the thermal convection current dual function of nitrogen and heating coil, material within inner draft tube flows downward, form inside and outside stream circulation, (2) at high temperature there is esterification in PTA powder and ethylene glycol room in esterification, and in esterification, the gauge pressure of room is 0.5～2bar, and the gaseous substance that esterification produces is discharged from room gaseous phase outlet esterification, along with new material constantly enters, the material reacted enters esterification discharging annular groove from external flow guiding cylinder material outlet, in esterification discharging annular groove, flowing one week continuation are heated and make reaction thorough, last from esterification material outlet discharge, carboxylate discharge nozzle is entered by esterifying liquid level control valve, the aperture of esterifying liquid level control valve is controlled by the liquid level of esterification discharging annular groove, and auxiliary agent is added in carboxylate discharge nozzle, (3) under the effect of potential difference and pressure reduction, being esterified material and auxiliary agent enters preheater and through material distribution plate, ethylene glycol gasification excessive in auxiliary agent produces bubble, and bubble moves upward and promotes material and stir, it is upwardly under precondensation after esterification material is heated room, (4) under precondensation, in room, material upwards sequentially passes through each floor tower tray and proceeds partial esterification reaction, and enters polycondensation process, when through tower tray, 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, forms air cavity at the top of material deflector cup, under precondensation, the absolute pressure in ceiling portion is 1～10kpa, vacuum in most last layer material deflector cup air cavity is the highest, more down progressively successively decrease, material degree of polymerization in process from bottom to top incrementally increases, enter polymer discharge annular groove, polymer discharge annular groove flow one week and continues heated, finally discharging from polymer discharge mouth, enter polymer discharge pipe by precondensation fluid level control valve.
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