CN112194782A - Device and method for producing PBT synthetic resin - Google Patents
Device and method for producing PBT synthetic resin Download PDFInfo
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- CN112194782A CN112194782A CN202011185014.7A CN202011185014A CN112194782A CN 112194782 A CN112194782 A CN 112194782A CN 202011185014 A CN202011185014 A CN 202011185014A CN 112194782 A CN112194782 A CN 112194782A
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- 229920003002 synthetic resin Polymers 0.000 title claims abstract description 47
- 239000000057 synthetic resin Substances 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- 238000005886 esterification reaction Methods 0.000 claims abstract description 67
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 52
- 239000002002 slurry Substances 0.000 claims abstract description 48
- 238000002156 mixing Methods 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000011268 mixed slurry Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000000155 melt Substances 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 12
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- 230000009467 reduction Effects 0.000 claims abstract description 6
- 238000004064 recycling Methods 0.000 claims abstract description 5
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 75
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 46
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 46
- 238000010438 heat treatment Methods 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 26
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000005507 spraying Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 13
- 230000032050 esterification Effects 0.000 claims description 12
- 238000006722 reduction reaction Methods 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 230000005484 gravity Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 6
- 230000018044 dehydration Effects 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 4
- 230000003014 reinforcing effect Effects 0.000 claims description 4
- 238000010793 Steam injection (oil industry) Methods 0.000 claims description 3
- 238000006482 condensation reaction Methods 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 3
- 229920001707 polybutylene terephthalate Polymers 0.000 description 36
- 238000010586 diagram Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- -1 polybutylene terephthalate Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- C08G63/785—Preparation processes characterised by the apparatus used
-
- 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
Abstract
The invention provides a device and a method for producing PBT synthetic resin, wherein the device comprises a slurry mixing device, an esterification reaction kettle, a pre-shrinking reaction kettle and a final shrinking reaction kettle which are connected in sequence; the slurry mixing device is used for mixing PTA and BDO, the mixed slurry is subjected to esterification reaction in the esterification reaction kettle, is subjected to preshrinking reaction in the preshrinking reaction kettle, and is finally subjected to final shrinkage reaction in the final shrinkage reaction kettle; the method comprises the following steps: step S001, preparing slurry; step S002, esterification reaction; step S003, pre-polycondensation reaction; step S004, performing final polycondensation reaction; step S005, granulating and packaging the melt; according to the device and the method for producing the PBT synthetic resin, provided by the invention, each reaction kettle in the device has the advantages of high reaction efficiency, good controllability, low energy consumption, high overall automation degree, continuous production and high production efficiency; the method has the advantages of simple process flow, high production efficiency, capability of recycling materials, reduction of device loss and good practicability.
Description
Technical Field
The invention relates to the field of PBT synthetic resin, in particular to a device and a method for producing PBT synthetic resin.
Background
The PBT is fully called polybutylene terephthalate, is a crystalline thermoplastic resin, has a melting point of 224-227 ℃, a relative density of 1.31-1.73 and an extremely low water absorption rate of 0.07 percent, has high mechanical strength, small friction coefficient and excellent self-lubricating property, and has the mechanical properties of tensile strength, elastic modulus and the like similar to those of engineering plastics such as polyformaldehyde, nylon and the like. Due to the above characteristics, PBT has been widely used in the automotive and electronic appliance industries. As the consumption of PBT increases, higher requirements are put on the performance of the PBT, and various new modification and processing technologies and new products are developed in developed countries and regions of the world in the year. The existing PBT synthetic resin production equipment has the disadvantages of complex structure, complex process flow, low reactor efficiency, poor controllability and high energy consumption, so the existing PBT synthetic resin production equipment needs to be improved.
Disclosure of Invention
Technical problem to be solved
The invention aims to solve the problem of providing a device and a method for producing PBT synthetic resin, so as to overcome the defects of low production efficiency and complicated process flow of the conventional PBT synthetic resin.
(II) technical scheme
In order to solve the technical problem, the invention provides a device for producing PBT synthetic resin, which comprises a slurry mixing device, an esterification reaction kettle, a pre-shrinking reaction kettle and a final shrinking reaction kettle which are sequentially connected; the slurry mixing device is used for mixing PTA and BDO, the mixed slurry is subjected to esterification reaction in the esterification reaction kettle, is subjected to preshrinking reaction in the preshrinking reaction kettle, and is finally subjected to final shrinkage reaction in the final shrinkage reaction kettle; :
the slurry mixing device comprises a slurry mixing tank, a PTA (pure terephthalic acid) bin and a chain scraper conveyor; a PTA inlet and a BDO inlet are arranged above the slurry mixing tank, and a mixed slurry outlet is arranged below the slurry mixing tank; the PTA bin is connected with the PTA inlet, the chain scraper conveyor is connected with the PTA bin, and the BDO inlet is connected with the BDO recovery tank;
the esterification reaction kettle comprises an esterification reaction kettle body; a slurry inlet connected with the mixed slurry outlet is arranged above the esterification reaction kettle body; an annular baffle is arranged in the esterification reaction kettle body and divides an inner cavity of the esterification reaction kettle body into an inner chamber and an outer chamber; a baffle is arranged in the outer chamber, an inner chamber channel and an outer chamber channel are arranged at the upper part of the annular baffle, an esterified substance outlet is arranged at the side end of the esterification reaction kettle body, and the esterified substance outlet and the inner chamber channel and the outer chamber channel are respectively arranged at two sides of the baffle;
the pre-shrinking reaction kettle comprises a pre-shrinking reaction kettle body; an annular trough is arranged in the pre-shrinking reaction kettle body and divides an inner cavity of the pre-shrinking reaction kettle body into an upper chamber and a lower chamber; a pre-shrinking feed inlet connected with the esterified product outlet is formed in the middle section of the pre-shrinking reaction kettle body, the pre-shrinking feed inlet is communicated with the bottom of the upper chamber, an overflow port is formed in the annular material groove, and a pre-shrinking discharge port is formed in the center of the bottom of the pre-shrinking reaction kettle body;
the final reduction reaction kettle comprises a final reduction reaction kettle body; and a final shrinkage feed inlet connected with the pre-shrinkage discharge outlet is formed in one side of the front end of the final shrinkage reaction kettle body, a final shrinkage discharge outlet is formed in the lower side of the rear end of the final shrinkage reaction kettle body, and a disc stirring device is installed in the final shrinkage reaction kettle body.
Further, an inner cylinder is arranged at the center of the lower side of the inner chamber, and a tube array heater is sleeved outside the inner cylinder; the tubular heater includes the inner tube that heating cauldron body and a plurality of edge circumferencial direction set up, the inner tube is vertical and link up the setting, be provided with first heat medium import and first heat medium export on the heating cauldron body respectively. A stirrer mounting opening is formed in the center of the upper side of the esterification reaction kettle body; the stirrer mounting port is provided with a gas phase outlet on the left side, and is provided with the slurry inlet on the right side, and the slurry inlet is provided with a material guide pipe.
Further, a stirring device is arranged in the lower chamber, and a heating coil is arranged on the periphery of the stirring device; the heating coil is provided with second heat medium inlet pipe and second heat medium outlet pipe respectively, the second heat medium inlet pipe is followed the lateral wall of preshrinking reation kettle body stretches out, the second heat medium outlet pipe is followed the bottom of preshrinking reation kettle body stretches out.
Furthermore, a disc rotating shaft is arranged at the center of the disc stirring device, one end of the disc rotating shaft extends to the outside of the final reduction reaction kettle body, the other end of the disc rotating shaft is supported on a support frame, and the support frame is fixed on the inner wall of the final reduction reaction kettle body. The disc rotating shaft is provided with a plurality of disc sets along the axial direction, each disc set comprises a plurality of discs, each disc is fixedly connected with the disc rotating shaft through a reinforcing rib plate, and the outer edges of the discs are connected into a whole through connecting pins.
The invention also provides a method for producing the PBT synthetic resin, which comprises the following steps:
step S001, preparing slurry; conveying and unloading PTA powder into a bin of a chain scraper conveyor, conveying the PTA powder into the PTA bin by the chain scraper conveyor, continuously and uniformly adding the PTA powder stored in the PTA bin into a slurry mixing tank downwards through an adjustable rotary valve by means of gravity, and then extracting BDO from a BDO recovery tank into the slurry mixing tank; preparing PTA and BDO into mixed slurry with a molar ratio of 1.2-1.4 in the slurry mixing tank;
step S002, esterification reaction; conveying the mixed slurry into an esterification reaction kettle through a conveying pump, allowing the mixed slurry to enter an inner chamber from a slurry inlet, and performing esterification reaction under the conditions of pressure of-60 kPa, temperature of 240-250 ℃ and stirring; the liquid phase material enters the tubular heater under the driving force formed by the pressure difference and the density difference of the double-chamber structure, then enters the outer chamber through the inner chamber channel and the outer chamber channel, circularly flows for a circle in the outer chamber, and then flows out from the esterification product outlet to enter the oligomer pipeline; one part of the materials entering the oligomer pipeline enters the pre-polycondensation reaction kettle after passing through an oligomer homogenizer, and the other part of the materials flows back to the outer chamber after being injected with a catalyst;
step S003, pre-polycondensation reaction; the low polymer enters an annular upper chamber from a pre-shrinking feed inlet on the side surface of the pre-polycondensation reaction kettle, overflows into a lower chamber through an overflow port, a catalyst is added into the lower chamber, further esterification and polycondensation reactions are carried out under the conditions that the pressure is-98.5 kPa, the temperature is 240-250 ℃ and stirring is carried out, and the generated prepolymer enters a final-shrinking reaction kettle after passing through a prepolymer filter;
step S004, performing final polycondensation reaction; the prepolymer enters from a final shrinkage feed inlet at the bottom of the final shrinkage reaction kettle, the final polycondensation reaction is carried out under the conditions that the pressure is-99.9 kPa, the temperature is 245 ℃ and the stirring of a disc stirring device is carried out, and after the generated final polymer stays in the final shrinkage reaction kettle for a certain time, the polycondensate melt meeting the product index requirement is pumped out from a final shrinkage discharge port by a discharge pump;
step S005, granulating and packaging the melt; the PBT synthetic resin melt from the final shrinkage discharge port is pumped out by the melt discharge pump, the melt discharge pump controls a certain rotating speed according to the yield to pressurize and discharge the PBT synthetic resin melt, the viscosity is measured by a viscometer, the reaction pressure of the final shrinkage reaction kettle is timely adjusted, and then the PBT synthetic resin melt enters a melt filter to remove condensed particles with the particle size of more than 20 mu m; and conveying the filtered melt to a belt casting and granulating system, casting a belt, granulating, weighing and packaging after granulating.
Further, the method also comprises the following steps:
step S006, separating esterification steam; in the esterification reaction, generated esterification steam enters a separation tower from a gas phase outlet at the top of an esterification reaction kettle for separation, the steam flows upwards through tower trays after entering from the bottom of the separation tower and exchanges heat with liquid flowing back from the upper layer of the tower trays, mixed steam discharged from the top of the separation tower enters a tower top condenser and is directly condensed by cooling water, and steam condensate cooled by the tower top condenser flows into a mixed liquid reflux tank by means of gravity; in the mixed liquid reflux tank, part of the condensate is returned to the top of the separation tower through a reflux pump, and the rest of the condensate is conveyed to a crude tetrahydrofuran aqueous solution storage tank.
Step S007, recycling THF; and (2) introducing the crude tetrahydrofuran aqueous solution into a dehydration tower, a de-LB tower and a de-HB tower in sequence, rectifying the crude tetrahydrofuran aqueous solution in the dehydration tower at normal pressure, rectifying the crude tetrahydrofuran aqueous solution in the de-LB tower at high pressure, refining the crude tetrahydrofuran aqueous solution in the de-HB tower at normal pressure, and storing THF removed from the de-HB tower in a THF intermediate tank.
Step S008, vacuum spraying; introducing the gas phase in the pre-polycondensation reaction and the gas phase in the final polycondensation reaction into a vacuum spraying system; the condensation steam from the pre-polycondensation kettle enters a spray condenser and is sprayed by low-temperature circulating BDO, a large amount of 1, 4-butanediol in the steam is collected, and the condensed 1, 4-butanediol and the sprayed 1, 4-butanediol are collected into a pre-polycondensation BDO hot well together; most BDO in the pre-condensation heat well passes through a pre-condensation BDO pump and a BDO filter, is cooled by a BDO cooler and then returns to the spray condenser for spraying, and the tail gas which cannot be condensed is pumped away by a BDO steam injection vacuum system; and (3) spraying the polycondensation steam from the final polycondensation kettle through low-temperature circulating BDO in a final polycondensation spraying condenser to collect a large amount of BDO in the polycondensation steam, and allowing the condensate to flow back to a final polycondensation BDO hot well by virtue of gravity.
(III) advantageous effects
The device and the method for producing the PBT synthetic resin provided by the invention form a low-temperature short-process plug flow tower type PBT synthetic resin system by combining the advantages of a double-chamber external circulation tube heating esterification reaction kettle, a circulation overflow type double-chamber pre-polycondensation reaction kettle and a horizontal basket type film-forming final polycondensation reaction kettle, and each reaction kettle has high reaction efficiency, good controllability, low energy consumption, high integral automation degree, continuous production and high production efficiency; the method has the advantages of simple process flow, high production efficiency, capability of recycling materials, reduction of device loss and good practicability.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus for producing a PBT synthetic resin according to the present invention;
FIG. 2 is a schematic structural view of a slurry mixing apparatus for an apparatus for producing a PBT synthetic resin according to the present invention;
FIG. 3 is a schematic structural diagram of an esterification reaction kettle of an apparatus for producing PBT synthetic resin according to the invention;
FIG. 4 is a schematic structural diagram of an esterification reaction kettle of an apparatus for producing PBT synthetic resin according to another angle;
FIG. 5 is a schematic structural view of a tubular heater of an apparatus for producing a PBT synthetic resin according to the present invention;
FIG. 6 is a schematic structural diagram of a preshrinking reaction kettle of an apparatus for producing PBT synthetic resin according to the invention;
FIG. 7 is a schematic structural view of an annular trough of an apparatus for producing PBT synthetic resin according to the present invention;
FIG. 8 is a schematic structural diagram of a final reduction reaction kettle of a device for producing PBT synthetic resin;
FIG. 9 is a schematic structural view of a disk stirring apparatus for an apparatus for producing a PBT synthetic resin according to the present invention;
FIG. 10 is a schematic process flow diagram of a process for producing a PBT synthetic resin according to the invention;
the corresponding part names for the various reference numbers in the figures are: 1. a slurry mixing tank; 2. a PTA bunker; 3. a chain scraper conveyor; 4. a PTA inlet; 5. a BDO inlet; 6. a mixed slurry outlet; 7. a BDO recovery tank; 8. an esterification reaction kettle; 9. an esterification reaction kettle body; 10. a slurry inlet; 11. an annular baffle; 12. an inner chamber; 13. an outer chamber; 14. a baffle plate; 15. an inner and outer chamber channel; 16. an esterified product outlet; 17. pre-shrinking a reaction kettle; 18. pre-shrinking the reaction kettle body; 19. an annular trough; 20. an upper chamber; 21. a lower chamber; 22. pre-shrinking the feed inlet; 23. an overflow port; 24. pre-shrinking a discharge hole; 25. a final condensation reaction kettle; 26. a final shrinkage reaction kettle body; 27. a final reduction feed inlet; 28. a final shrinkage discharge hole; 29. a disc stirring device; 30. an inner barrel; 31. a tubular heater; 32. heating the kettle body; 33. an inner tube; 34. a first heating medium inlet; 35. a first heating medium outlet; 36. a stirrer mounting port; 37. a gas phase outlet; 38. a material guide pipe; 39. a heating coil; 40. a second heating medium inlet pipe; 41. a second heating medium outlet pipe; 42. a disk rotating shaft; 43. a support frame; 44. a disc; 45. reinforcing rib plates; 46. and (7) connecting pins.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Referring to fig. 1 to 9, the present invention provides an apparatus for producing PBT synthetic resin, comprising a slurry mixing device, an esterification reaction kettle 8, a pre-shrinking reaction kettle 17 and a final shrinking reaction kettle 25, which are connected in sequence; the slurry mixing device is used for mixing PTA and BDO, the mixed slurry is subjected to esterification reaction in the esterification reaction kettle 8, then is subjected to preshrinking reaction in the preshrinking reaction kettle 17, and finally is subjected to final shrinkage reaction in the final shrinkage reaction kettle 25;
referring to fig. 2, the slurry mixing apparatus includes a slurry mixing tank 1, a PTA (terephthalic acid) bin 2, and a chain scraper conveyor 3; a PTA inlet 4 and a BDO (1, 4-butanediol) inlet 5 are arranged above the slurry mixing tank 1, and a mixed slurry outlet 6 is arranged below the slurry mixing tank; the PTA bin 2 is connected with the PTA inlet 4, the chain plate conveyor 3 is connected with the PTA bin 2, and the BDO inlet 5 is connected with the BDO recovery tank 7;
referring to fig. 3 to 5, esterification reaction tank 8 includes esterification reaction tank body 9; a slurry inlet 10 connected with the mixed slurry outlet 6 is arranged above the esterification reaction kettle body 9; an annular baffle 11 is arranged in the esterification reaction kettle body 9, and the inner cavity of the esterification reaction kettle body 9 is divided into an inner chamber 12 and an outer chamber 13 by the annular baffle 11; a baffle plate 14 is arranged in the outer chamber 13, an inner chamber channel and an outer chamber channel 15 are arranged at the upper part of the annular baffle plate 11, an esterified substance outlet 16 is arranged at the side end of the esterification reaction kettle body 9, and the esterified substance outlet 16 and the inner chamber channel and the outer chamber channel 15 are respectively arranged at two sides of the baffle plate 14.
Wherein, an inner cylinder 30 is arranged at the center of the lower side of the inner chamber 12, and a tubular heater 31 is sleeved outside the inner cylinder 30; the tubular heater 31 includes a heating kettle body 32 and a plurality of inner tubes 33 arranged along the circumferential direction, the inner tubes 33 are vertically arranged in a penetrating manner, and a first heating medium inlet 34 and a first heating medium outlet 35 are respectively arranged on the heating kettle body 32. A stirrer mounting port 36 is arranged at the center of the upper side of the esterification reaction kettle body 9; the stirrer mounting port 36 is provided with a gas phase outlet 37 on the left side, a slurry inlet 10 on the right side, and a material guide pipe 38 is mounted on the slurry inlet 10.
Referring to fig. 6 and 7, the pre-shrinking reaction kettle 17 includes a pre-shrinking reaction kettle body 18; an annular trough 19 is arranged in the pre-shrinking reaction kettle body 18, and the annular trough 19 divides the inner cavity of the pre-shrinking reaction kettle body 18 into an upper chamber 20 and a lower chamber 21; the middle section of the pre-shrinking reaction kettle body 18 is provided with a pre-shrinking feed inlet 22 connected with the esterified product outlet 16, the pre-shrinking feed inlet 22 is communicated with the bottom of the upper chamber 20, the annular trough 19 is provided with an overflow port 23, and the center of the bottom of the pre-shrinking reaction kettle body 18 is provided with a pre-shrinking discharge port 24.
Wherein, a stirring device is arranged in the lower chamber 21, and a heating coil 39 is arranged on the periphery of the stirring device; a second heating medium inlet pipe 40 and a second heating medium outlet pipe 41 are respectively arranged on the heating coil 39, the second heating medium inlet pipe 40 extends out from the side wall of the pre-shrinking reaction kettle body 18, and the second heating medium outlet pipe 41 extends out from the bottom of the pre-shrinking reaction kettle body 18.
Referring to fig. 8 and 9, the finishing reaction tank 25 includes a finishing reaction tank body 26; a final shrinkage feed inlet 27 connected with the pre-shrinkage discharge outlet 24 is formed in one side of the front end of the final shrinkage reaction kettle body 26, a final shrinkage discharge outlet 28 is formed in the lower side of the rear end of the final shrinkage reaction kettle body 26, and a disc stirring device 29 is installed in the final shrinkage reaction kettle body 26.
Wherein, the center of the disc stirring device 29 is provided with a disc rotating shaft 42, one end of the disc rotating shaft 42 extends to the outside of the final-shrinkage reaction kettle body 26, the other end is supported on a supporting frame 43, and the supporting frame 43 is fixed on the inner wall of the final-shrinkage reaction kettle body 26. The disc rotating shaft 42 is provided with a plurality of disc sets along the axial direction, each disc set comprises a plurality of discs 44, the discs 44 are fixedly connected with the disc rotating shaft 42 through reinforcing rib plates 45, and the outer edges of the discs 44 are connected into a whole through connecting pins 46.
Referring to fig. 10, the present example also provides a method for producing PBT synthetic resin, including the steps of:
step S001, preparing slurry; the method comprises the following steps of conveying and discharging PTA (terephthalic acid) powder into a bin of a chain plate conveyor 3, conveying the PTA powder into a PTA bin 2 by the chain plate conveyor 3, continuously and uniformly adding the PTA powder stored in the PTA bin 2 into a slurry mixing tank 1 downwards through an adjustable rotary valve by means of gravity, and then extracting BDO (1, 4-butanediol) into the slurry mixing tank 1 from a BDO recovery tank 7; in a slurry mixing tank 1, preparing PTA and BDO into mixed slurry with a molar ratio of 1.2-1.4;
step S002, esterification reaction; conveying the mixed slurry into an esterification reaction kettle 8 through a conveying pump, allowing the mixed slurry to enter an inner chamber 12 from a slurry inlet 10, and performing esterification reaction under the conditions of pressure of-60 kPa, temperature of 240-250 ℃ and stirring; the liquid phase material enters the tubular heater 31 under the driving force formed by the pressure difference and the density difference of the double-chamber structure, then enters the outer chamber 13 through the inner chamber channel 15, circularly flows for a circle in the outer chamber 13, and then flows out from the esterification product outlet 16 to enter the oligomer pipeline; one part of the materials entering the oligomer pipeline enters the pre-polycondensation reaction kettle 17 after passing through an oligomer homogenizer, and the other part of the materials flows back to the outer chamber 13 after being injected with a catalyst; in this embodiment, the catalyst may be tetrabutyl titanate.
Step S003, pre-polycondensation reaction; the oligomer enters an annular upper chamber 20 from a pre-shrinking feed inlet 22 on the side surface of a pre-polycondensation reaction kettle 17, overflows into a lower chamber 21 through an overflow port 23, a catalyst is added into the lower chamber 21, further esterification and polycondensation reactions are carried out under the conditions that the pressure is-98.5 kPa, the temperature is 240-250 ℃ and stirring is carried out, and the generated prepolymer enters a final-shrinking reaction kettle 25 after passing through a prepolymer filter;
step S004, performing final polycondensation reaction; the prepolymer enters from a final shrinkage feed inlet 27 at the bottom of a final shrinkage reaction kettle 25, the final polycondensation reaction is carried out under the conditions that the pressure is-99.9 kPa, the temperature is 245 ℃ and the stirring is carried out by a disc stirring device 29, and after the generated final polymer stays in the final shrinkage reaction kettle 25 for a certain time, a polycondensate melt meeting the product index requirement is pumped out from a final shrinkage discharge outlet 28 by a discharge pump;
step S005, granulating and packaging the melt; the PBT synthetic resin melt from the final shrinkage discharge port 28 is pumped out by a melt discharge pump, the melt discharge pump controls a certain rotating speed according to the yield to pressurize and discharge the PBT synthetic resin melt, the viscosity is measured by a viscometer, the reaction pressure of the final shrinkage reaction kettle 25 is timely adjusted, and then the PBT synthetic resin melt enters a melt filter to remove condensed particles with the particle size of more than 20 mu m; and conveying the filtered melt to a belt casting and granulating system, casting a belt, granulating, weighing and packaging after granulating.
In order to make the process more complete, the method also comprises the following steps:
step S006, separating esterification steam; in the esterification reaction, the generated esterification steam enters a separation tower from a gas phase outlet 37 at the top of an esterification reaction kettle 8 for separation, the steam flows upwards through tower trays after entering from the bottom of the separation tower and exchanges heat with liquid flowing back from the upper layer of the tower trays, mixed steam discharged from the top of the separation tower enters a tower top condenser and is directly condensed by cooling water, and steam condensate cooled by the tower top condenser flows into a mixed liquid reflux tank by gravity; in the mixed liquid reflux tank, part of the condensate is returned to the top of the separating tower through a reflux pump, and the rest of the condensate is conveyed to a crude tetrahydrofuran aqueous solution storage tank.
Step S007, recovery of THF (tetrahydrofuran); and (2) introducing the crude tetrahydrofuran aqueous solution into a dehydration tower, a dehydro-LB tower and a dehydro-HB tower in sequence, rectifying the crude tetrahydrofuran aqueous solution in the dehydration tower at normal pressure, rectifying the crude tetrahydrofuran aqueous solution in the dehydro-LB tower under pressure, refining the crude tetrahydrofuran aqueous solution in the dehydro-HB tower at normal pressure, and storing THF (tetrahydrofuran) separated from the dehydro-HB tower in a THF intermediate tank.
Step S008, vacuum spraying; introducing the gas phase in the pre-polycondensation reaction and the gas phase in the final polycondensation reaction into a vacuum spraying system; the condensation steam from the pre-polycondensation kettle enters a spray condenser and is sprayed by low-temperature circulating BDO, a large amount of 1, 4-butanediol in the steam is collected, and the condensed 1, 4-butanediol and the sprayed 1, 4-butanediol are collected into a pre-polycondensation BDO hot well together; most BDO in the pre-condensation heat well passes through a pre-condensation BDO pump and a BDO filter, is cooled by a BDO cooler and then returns to the spray condenser for spraying, and the tail gas which cannot be condensed is pumped away by a BDO steam injection vacuum system; and (3) spraying the polycondensation steam from the final polycondensation kettle through low-temperature circulating BDO in a final polycondensation spraying condenser to collect a large amount of BDO in the polycondensation steam, and allowing the condensate to flow back to a final polycondensation BDO hot well by virtue of gravity.
In the device and the method for producing the PBT synthetic resin, the device forms a low-temperature short-process plug flow tower type PBT synthetic resin system by combining the advantages of a double-chamber external circulation tube heating esterification reaction kettle, a circulation overflow type double-chamber pre-polycondensation reaction kettle and a horizontal basket type film-forming final polycondensation reaction kettle, and each reaction kettle has high reaction efficiency, good controllability, low energy consumption, high integral automation degree, continuous production and high production efficiency; the method has the advantages of simple process flow, high production efficiency, capability of recycling materials, reduction of device loss and good practicability.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. An apparatus for producing a PBT synthetic resin, characterized in that: comprises a slurry mixing device, an esterification reaction kettle (8), a pre-shrinking reaction kettle (17) and a final shrinking reaction kettle (25) which are connected in sequence; the slurry mixing device is used for mixing PTA and BDO, the mixed slurry is subjected to esterification reaction in the esterification reaction kettle (8), is subjected to pre-shrinking reaction in the pre-shrinking reaction kettle (17), and is finally subjected to final shrinking reaction in the final shrinking reaction kettle (25);
the slurry mixing device comprises a slurry mixing tank (1), a PTA (pure terephthalic acid) bin (2) and a chain scraper conveyor (3); a PTA inlet (4) and a BDO inlet (5) are arranged above the slurry mixing tank (1), and a mixed slurry outlet (6) is arranged below the slurry mixing tank; the PTA bin (2) is connected with the PTA inlet (4), the chain plate conveyor (3) is connected with the PTA bin (2), and the BDO inlet (5) is connected with the BDO recovery tank (7);
the esterification reaction kettle (8) comprises an esterification reaction kettle body (9); a slurry inlet (10) connected with the mixed slurry outlet (6) is arranged above the esterification reaction kettle body (9); an annular baffle (11) is arranged in the esterification reaction kettle body (9), and the annular baffle (11) divides an inner cavity of the esterification reaction kettle body (9) into an inner chamber (12) and an outer chamber (13); a baffle (14) is arranged in the outer chamber (13), an inner chamber channel and an outer chamber channel (15) are arranged at the upper part of the annular baffle (11), an esterified substance outlet (16) is arranged at the side end of the esterification reaction kettle body (9), and the esterified substance outlet (16) and the inner chamber channel and the outer chamber channel (15) are respectively arranged at two sides of the baffle (14);
the pre-shrinking reaction kettle (17) comprises a pre-shrinking reaction kettle body (18); an annular trough (19) is arranged in the pre-shrinking reaction kettle body (18), and the annular trough (19) divides the inner cavity of the pre-shrinking reaction kettle body (18) into an upper chamber (20) and a lower chamber (21); a pre-shrinking feed inlet (22) connected with the esterified product outlet (16) is formed in the middle section of the pre-shrinking reaction kettle body (18), the pre-shrinking feed inlet (22) is communicated with the bottom of the upper chamber (20), an overflow port (23) is formed in the annular trough (19), and a pre-shrinking discharge port (24) is formed in the center of the bottom of the pre-shrinking reaction kettle body (18);
the final condensation reaction kettle (25) comprises a final condensation reaction kettle body (26); a final shrinkage feed inlet (27) connected with the pre-shrinkage discharge outlet (24) is formed in one side of the front end of the final shrinkage reaction kettle body (26), a final shrinkage discharge outlet (28) is formed in the lower side of the rear end of the final shrinkage reaction kettle body (26), and a disc stirring device (29) is installed in the final shrinkage reaction kettle body (26).
2. The apparatus for producing a PBT synthetic resin according to claim 1, wherein: an inner cylinder (30) is arranged at the center of the lower side of the inner chamber (12), and a tube array heater (31) is sleeved outside the inner cylinder (30); the shell and tube heater (31) is including heating cauldron body (32) and a plurality of inner tube (33) that set up along the circumferencial direction, inner tube (33) are vertical and link up the setting, be provided with first heat medium import (34) and first heat medium export (35) on heating cauldron body (32) respectively.
3. The apparatus for producing a PBT synthetic resin according to claim 1, wherein: a stirrer mounting opening (36) is formed in the center of the upper side of the esterification reaction kettle body (9); the stirrer mounting port (36) is provided with a gas phase outlet (37) on the left side, the slurry inlet (10) on the right side, and the slurry inlet (10) is provided with a material guide pipe (38).
4. The apparatus for producing a PBT synthetic resin according to claim 1, wherein: a stirring device is arranged in the lower chamber (21), and a heating coil (39) is arranged on the periphery of the stirring device; be provided with second heat medium inlet pipe (40) and second heat medium outlet pipe (41) on heating coil (39) respectively, second heat medium inlet pipe (40) are followed the lateral wall of preshrinking reation kettle body (18) stretches out, second heat medium outlet pipe (41) are followed the bottom of preshrinking reation kettle body (18) stretches out.
5. The apparatus for producing a PBT synthetic resin according to claim 1, wherein: the center of the disc stirring device (29) is provided with a disc rotating shaft (42), one end of the disc rotating shaft (42) extends to the outside of the final-shrinkage reaction kettle body (26), the other end of the disc rotating shaft is supported on a supporting frame (43), and the supporting frame (43) is fixed on the inner wall of the final-shrinkage reaction kettle body (26).
6. The apparatus for producing a PBT synthetic resin according to claim 5, wherein: the disc rotating shaft (42) is provided with a plurality of disc sets along the axial direction, each disc set comprises a plurality of discs (44), each disc (44) is fixedly connected with the disc rotating shaft (42) through a reinforcing rib plate (45), and the outer edges of the discs (44) are connected into a whole through connecting pins (46).
7. A process for producing a PBT synthetic resin, comprising the steps of:
step S001, preparing slurry; conveying and unloading PTA powder into a bin of a chain scraper conveyor (3), conveying the PTA powder into a PTA bin (2) by the chain scraper conveyor (3), continuously and uniformly adding the PTA powder stored in the PTA bin (2) into a slurry mixing tank (1) downwards by virtue of gravity through an adjustable rotary valve, and then extracting BDO from a BDO recovery tank (7) into the slurry mixing tank (1); in the slurry mixing tank (1), preparing PTA and BDO into mixed slurry with a molar ratio of 1.2-1.4;
step S002, esterification reaction; conveying the mixed slurry into an esterification reaction kettle (8) through a conveying pump, feeding the mixed slurry into an inner chamber (12) from a slurry inlet (10), and carrying out esterification reaction under the conditions of pressure of-60 kPa, temperature of 240-250 ℃ and stirring; the liquid phase material enters a tube heater (31) under the driving force formed by the pressure difference and the density difference of a double-chamber structure, then enters an outer chamber (13) through an inner chamber channel (15) and an outer chamber channel (13), circularly flows for a circle in the outer chamber (13), and then flows out from an esterification product outlet (16) and enters an oligomer pipeline; one part of the material entering the oligomer pipeline enters a pre-polycondensation reaction kettle (17) after passing through an oligomer homogenizer, and the other part of the material returns to the outer chamber (13) after being injected with a catalyst;
step S003, pre-polycondensation reaction; the oligomer enters an annular upper chamber (20) from a pre-shrinking feed port (22) on the side surface of the pre-polycondensation reaction kettle (17), overflows into a lower chamber (21) through an overflow port (23), a catalyst is added into the lower chamber (21), further esterification and polycondensation reactions are carried out under the conditions that the pressure is-98.5 kPa, the temperature is 240-250 ℃ and stirring is carried out, and the generated prepolymer enters a final polycondensation reaction kettle (25) after passing through a prepolymer filter;
step S004, performing final polycondensation reaction; the prepolymer enters from a final reduction feed inlet (27) at the bottom of the final reduction reaction kettle (25), the final polycondensation reaction is carried out under the conditions that the pressure is-99.9 kPa, the temperature is 245 ℃ and the stirring of a disc stirring device (29) is carried out, after the generated final polymer stays in the final reduction reaction kettle (25) for a certain time, the polycondensate melt meeting the product index requirement is pumped out from a final reduction discharge outlet (28) by a discharge pump;
step S005, granulating and packaging the melt; the PBT synthetic resin melt from the final shrinkage discharge hole (28) is pumped out by the melt discharge pump, the melt discharge pump controls a certain rotating speed according to the yield to pressurize and send out the PBT synthetic resin melt, the viscosity is measured by a viscometer, the reaction pressure of the final shrinkage reaction kettle (25) is timely adjusted, and then the PBT synthetic resin melt enters a melt filter to remove condensed particles with the particle size of more than 20 mu m; and conveying the filtered melt to a belt casting and granulating system, casting a belt, granulating, weighing and packaging after granulating.
8. The process for producing a PBT synthetic resin according to claim 7, further comprising the steps of:
step S006, separating esterification steam; in the esterification reaction, generated esterification steam enters a separation tower from a gas phase outlet (37) at the top of an esterification reaction kettle (8) for separation, the steam flows upwards through tower trays after entering from the bottom of the separation tower and exchanges heat with liquid flowing back from the upper layer of the tower trays, mixed steam discharged from the top of the separation tower enters a tower top condenser and is directly condensed by cooling water, and steam condensate cooled by the tower top condenser flows into a mixed liquid reflux tank by virtue of gravity; in the mixed liquid reflux tank, part of the condensate is returned to the top of the separation tower through a reflux pump, and the rest of the condensate is conveyed to a crude tetrahydrofuran aqueous solution storage tank.
9. The process for producing a PBT synthetic resin according to claim 8, further comprising the steps of:
step S007, recycling THF; and (2) introducing the crude tetrahydrofuran aqueous solution into a dehydration tower, a de-LB tower and a de-HB tower in sequence, rectifying the crude tetrahydrofuran aqueous solution in the dehydration tower at normal pressure, rectifying the crude tetrahydrofuran aqueous solution in the de-LB tower at high pressure, refining the crude tetrahydrofuran aqueous solution in the de-HB tower at normal pressure, and storing THF removed from the de-HB tower in a THF intermediate tank.
10. The process for producing a PBT synthetic resin according to claim 7, further comprising the steps of:
step S008, vacuum spraying; introducing the gas phase in the pre-polycondensation reaction and the gas phase in the final polycondensation reaction into a vacuum spraying system; the condensation steam from the pre-polycondensation kettle enters a spray condenser and is sprayed by low-temperature circulating BDO, a large amount of 1, 4-butanediol in the steam is collected, and the condensed 1, 4-butanediol and the sprayed 1, 4-butanediol are collected into a pre-polycondensation BDO hot well together; most BDO in the pre-condensation heat well passes through a pre-condensation BDO pump and a BDO filter, is cooled by a BDO cooler and then returns to the spray condenser for spraying, and the tail gas which cannot be condensed is pumped away by a BDO steam injection vacuum system; and (3) spraying the polycondensation steam from the final polycondensation kettle through low-temperature circulating BDO in a final polycondensation spraying condenser to collect a large amount of BDO in the polycondensation steam, and allowing the condensate to flow back to a final polycondensation BDO hot well by virtue of gravity.
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| CN202011185014.7A CN112194782A (en) | 2020-10-29 | 2020-10-29 | Device and method for producing PBT synthetic resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115746282A (en) * | 2022-10-28 | 2023-03-07 | 浙江长鸿生物材料有限公司 | Flexible switching production process of PBAT (poly (butylene adipate-co-terephthalate)) and PBT (polybutylene terephthalate) products |
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| CN109529753A (en) * | 2019-01-14 | 2019-03-29 | 扬州惠通化工科技股份有限公司 | A kind of PBT esterification system |
| CN213506696U (en) * | 2020-10-29 | 2021-06-22 | 浙江美源新材料股份有限公司 | Device for producing PBT synthetic resin |
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| CN103349947A (en) * | 2013-07-24 | 2013-10-16 | 江苏长乐纤维科技有限公司 | Feeding system for polyester production |
| US20170369638A1 (en) * | 2015-01-30 | 2017-12-28 | Sabic Global Technologies B.V. | Continuous process for making polybutylene terephthalate using purified terephthalic acid and 1,4-butane diol |
| CN109529753A (en) * | 2019-01-14 | 2019-03-29 | 扬州惠通化工科技股份有限公司 | A kind of PBT esterification system |
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