CN117398954A - Device and method for preparing polybutylene terephthalate - Google Patents
Device and method for preparing polybutylene terephthalate Download PDFInfo
- Publication number
- CN117398954A CN117398954A CN202211508569.XA CN202211508569A CN117398954A CN 117398954 A CN117398954 A CN 117398954A CN 202211508569 A CN202211508569 A CN 202211508569A CN 117398954 A CN117398954 A CN 117398954A
- Authority
- CN
- China
- Prior art keywords
- reaction
- kettle
- esterification
- melt
- final
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920001707 polybutylene terephthalate Polymers 0.000 title claims abstract description 28
- -1 polybutylene terephthalate Polymers 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- 238000005886 esterification reaction Methods 0.000 claims abstract description 37
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 230000032050 esterification Effects 0.000 claims abstract description 26
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 25
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 17
- 238000005507 spraying Methods 0.000 claims abstract description 13
- 239000011268 mixed slurry Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000007423 decrease Effects 0.000 claims 1
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 229920001896 polybutyrate Polymers 0.000 claims 1
- 238000009987 spinning Methods 0.000 abstract description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 6
- 229920000728 polyester Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 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 2
- 239000000463 material Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229920000180 alkyd Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Classifications
-
- 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
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
-
- 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
-
- 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
Abstract
The invention discloses a device and a method for preparing polybutylene terephthalate, wherein the device comprises the following steps: the method comprises the steps of sequentially carrying out esterification, pre-polycondensation and final polycondensation reactions on mixed slurry of terephthalic acid and 1, 4-butanediol in a device, wherein the catalyst enters the esterification kettle or the pre-polycondensation kettle from a catalyst adding port in a spraying manner, and the catalyst enters the polybutylene terephthalate with an average polymerization degree of 130-200 after the reaction is finished. The high molecular weight polybutylene terephthalate prepared by the specific device and method has high average polymerization degree, excellent spinning performance and heat stability.
Description
Technical Field
The invention relates to a device for preparing polyester and a using method thereof, in particular to a device for preparing polybutylene terephthalate and a using method thereof.
Background
Polybutylene terephthalate (PBT) is a crystalline thermoplastic polyester, has the advantages of excellent mechanical properties, heat resistance, solubility resistance and the like, and is one of five engineering plastics. The process for polymerizing PBT by direct esterification method uses refined terephthalic acid (PTA) and 1, 4-Butanediol (BDO) as raw materials, tetrabutyl titanate (TBT) as catalyst, and comprises three stages of esterification reaction, pre-polycondensation reaction and final polycondensation reaction, wherein the polymer PBT melt is generated under the control of temperature, pressure, residence time, stirring rotation speed and the like, and the PBT slice is finally produced by a granulating and packaging system. However, the prior art only gives PBT polyesters having an average degree of polymerization of from 70 to 130.
Disclosure of Invention
The invention aims to: in order to solve the technical problems in the prior art, the invention aims to provide a preparation device for preparing polybutylene terephthalate with stable and uniform catalyst feeding and high average polymerization degree, and also provides a method for preparing polybutylene terephthalate by using the device.
The technical scheme is as follows: the preparation device of the polybutylene terephthalate comprises: the esterification reactor, the preshrinking reactor and the final shrinking reactor are provided with common baffles and heating baffles which are alternately arranged at the inlet end of the final shrinking reactor, and a weir plate is arranged at the middle part of the common baffles.
Further, the height of the common baffle is 1.2-3.0 times of the height of the heating baffle, the distance between the common baffle and the heating baffle is in a proportional relation with the height of the common baffle, the height of the weir plate is in a descending trend from the inlet end to the inside, the front end can be ensured to finish tackifying reaction, a gradually tackified polymer passes through the weir plate and climbs through the heating baffle, the movement track of the polymer is in a sine curve shape, the middle part of the heating baffle is provided with a channel, the inside of the heating baffle is provided with baffle plates and high-temperature heat mediums, and the arrangement of the baffle plates can prevent the heat mediums from being short-circuited and ensure that the high-viscosity polymer flows uniformly.
Further, the preferable arrangement mode of the common baffle plate and the heating baffle plate is that the common baffle plate is alternately arranged at the two ends and the heating baffle plate is arranged in the middle.
The method for preparing polybutylene terephthalate by using the device comprises the following steps:
(a) Adding mixed slurry of terephthalic acid and 1, 4-butanediol into an esterification kettle for esterification reaction, and allowing a catalyst to enter the esterification kettle in a spraying manner through a catalyst adding port to react to obtain an esterification melt with an average polymerization degree of 5-20;
(b) Adding the esterified melt into a pre-shrinking kettle for pre-shrinking reaction to obtain pre-shrinking melt with the average polymerization degree of 30-60;
(c) Adding the pre-condensed melt into a final condensation kettle, tackifying the pre-condensed melt at the inlet end of the final condensation kettle by using common baffles and heating baffles which are alternately arranged, and then carrying out final polycondensation reaction to obtain a final condensed melt with the average polymerization degree of 130-200, preferably 135-195, so as to obtain the polybutylene terephthalate.
Further, in the step (a), the molar ratio of terephthalic acid to 1, 4-butanediol is 1:2.0-1:3.2.
Further, in the step (a), the esterification reaction conditions are as follows: the reaction temperature is 236-246 ℃, the reaction pressure is 35-55kPa, the residence time is 1.5-3.5h, and the rotation speed of the stirrer is 90-160rpm.
Further, in the step (a), after the catalyst and the fresh BDO are prepared, the catalyst enters the esterification kettle through a catalyst adding port in a spraying mode, the spraying speed is 10-30m/s, the adding mode can enable the adding amount of the catalyst to be more stable and uniformly dispersed in the kettle to effectively ensure the esterification reaction, and the catalyst is a titanium catalyst and is added in the esterification kettle independently or in batches in the esterification kettle and the preshrinking kettle.
Further, in the step (b), the conditions for the pre-polymerization reaction are as follows: the reaction temperature is 245-255 ℃, the reaction pressure is 1.0-3.0kPa, the residence time is 1.5-3.0h, and the rotation speed of the stirrer is 40-80rpm.
Further, in the step (c), the condition of the final polycondensation reaction is: the reaction temperature is 245-255 ℃, the reaction pressure is 40-150kPa, the residence time is 0.8-2.0h, and the rotation speed of the stirrer is 2-10rpm.
The principle of the invention: firstly, the invention sets a plurality of groups of special baffles at the inlet end of the final shrinking kettle to form a special runner for melt, the design of the special runner provides residence time and temperature required by tackifying, and simultaneously ensures the fluidity of the high molecular weight polymer, secondly, in the invention, the terephthalic acid and the 1, 4-butanediol are utilized to carry out alkyd esterification reaction in the esterification kettle to generate the terephthalic acid bis-4-hydroxybutyl ester, and then the polycondensation reaction is carried out between the terephthalic acid bis-4-hydroxybutyl ester molecules in two serially connected polycondensation kettles to remove butanediol molecules, thus finally obtaining the product with the polymerization degree of 130-200.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages:
(1) The polybutylene terephthalate produced by the three-kettle direct esterification method has the average polymerization degree of 130-200, and has the outstanding advantages of excellent spinning performance and high thermal stability compared with the polyester with low average polymerization degree in the prior art;
(2) The final shrinkage kettle has unique structural design, is provided with the common baffles and the heating baffles which are alternately arranged, and can ensure that the front end completes the tackifying reaction through the design of the height and the structure thereof;
(3) Compared with the traditional spraying type, the catalyst adding mode can ensure that the catalyst adding amount is more stable, the catalyst is more uniformly mixed with materials in a kettle, and the esterification reaction is effectively ensured;
(4) The process and the device adopted in the invention have short flow, greatly avoid the problem of waste products caused by thermal degradation of materials after long residence time in the kettle, and simultaneously reduce the waste of the recycled BDO with higher production efficiency.
Drawings
FIG. 1 is a schematic view of an apparatus for producing polybutylene terephthalate according to the present invention;
FIG. 2 is a schematic view of alternate baffles of the present invention;
FIG. 3 is a side view of a generic baffle of the present invention;
FIG. 4 is a side view of a heating baffle of the present invention.
Description of the drawings
The invention will be further illustrated with reference to specific examples.
The preparation device of the polybutylene terephthalate comprises an esterification kettle 1, a preshrinking kettle 2 and a final shrinking kettle 3 in sequence as shown in figure 1, wherein the final shrinking kettle 3 is provided with common baffles 31 and heating baffles 32 which are alternately arranged at the inlet end of the final shrinking kettle 3 as shown in figure 2, the preferable arrangement mode is that the common baffles 31 are alternately arranged at the two ends and the heating baffles 32 are arranged in the middle, the height of the common baffles 31 is 1.2-3.0 times of the height of the heating baffles 32, as shown in figure 3, the middle part of the common baffles 31 is provided with weir plates 33, the height of the weir plates 33 is in a descending trend from the inlet end to the inside, the front end is ensured to finish tackifying reaction, and a gradually tackified polymer passes through the weir plates 33 and climbs through the heating baffles 32, and the movement track of the polymer is in a sine curve; as shown in fig. 4, the middle part of the heating baffle 31 is provided with a channel 34, a baffle 35 and a high-temperature heating medium are arranged in the middle part, the arrangement of a plurality of baffles 34 can prevent the heating medium from being short-circuited, and the distance between the common baffle 31 and the heating baffle 32 is in direct proportion to the height of the common baffle 31.
Example 1: the application method of the device for preparing the polybutylene terephthalate comprises the following steps:
(a) Adding mixed slurry with the mol ratio of terephthalic acid to 1, 4-butanediol being 3.1 into an esterification kettle 1 for esterification reaction, wherein the reaction conditions are as follows: the reaction temperature is 238 ℃, the reaction pressure is 50kPa, the residence time is 2 hours, the rotation speed of a stirrer is 140rpm, and an esterified melt is obtained after the reaction is finished;
after the titanium catalyst and fresh BDO are prepared, the titanium catalyst enters the esterification kettle 1 through a catalyst adding port in a spraying mode, wherein the spraying speed is 20m/s;
(b) The esterified melt is added into a preshrinking kettle 2 from an outer chamber to carry out preshrinking reaction under the following conditions: the reaction temperature is 245 ℃, the reaction pressure is 2.0kPa, the residence time is 1.5 hours, the rotation speed of a stirrer is 60rpm, and the pre-polycondensed melt is obtained after the reaction is finished;
(c) The pre-polycondensation melt is produced from the inner chamber of the pre-polycondensation kettle and is added into the final polycondensation kettle 3, and after the pre-polycondensation melt is thickened by the common baffle plates 31 and the heating baffle plates 32 which are alternately arranged at the inlet end of the final polycondensation kettle 3, the final polycondensation reaction is carried out under the reaction conditions that: the reaction temperature is 250 ℃, the reaction pressure is 80kPa, the residence time is 1h, the rotation speed of a stirrer is 9.0rpm, and the final polycondensation melt is obtained after the reaction is finished, namely the polybutylene terephthalate.
Example 2: the application method of the device for preparing the polybutylene terephthalate comprises the following steps:
(a) Adding mixed slurry with the mol ratio of terephthalic acid to 1, 4-butanediol being 3.1 into an esterification kettle 1 for esterification reaction, wherein the reaction conditions are as follows: the reaction temperature is 238 ℃, the reaction pressure is 50kPa, the residence time is 2 hours, the rotation speed of a stirrer is 140rpm, and an esterified melt is obtained after the reaction is finished;
after the titanium catalyst and fresh BDO are prepared, the titanium catalyst enters the esterification kettle 1 through a catalyst adding port in a spraying mode, wherein the spraying speed is 20m/s;
(b) Adding the esterified melt into a pre-shrinking kettle 2 from an outer chamber to perform pre-shrinking reaction, wherein the reaction conditions are as follows: the reaction temperature is 245 ℃, the reaction pressure is 2.0kPa, the residence time is 1.5 hours, the rotation speed of a stirrer is 60rpm, and the pre-polycondensed melt is obtained after the reaction is finished;
(c) The pre-polycondensation melt is produced from the inner chamber of the pre-polycondensation kettle and is added into the final polycondensation kettle 3, and after the pre-polycondensation melt is thickened by the common baffle plates 31 and the heating baffle plates 32 which are alternately arranged at the inlet end of the final polycondensation kettle 3, the final polycondensation reaction is carried out under the reaction conditions that: the reaction temperature is 250 ℃, the reaction pressure is 80kPa, the residence time is 1h, the rotation speed of a stirrer is 7.5rpm, and the final polycondensation melt is obtained after the reaction is finished, namely the polybutylene terephthalate.
Example 3: the application method of the device for preparing the polybutylene terephthalate comprises the following steps:
(a) Adding mixed slurry with the mol ratio of terephthalic acid to 1, 4-butanediol being 3.1 into an esterification kettle 1 for esterification reaction, wherein the reaction conditions are as follows: the reaction temperature is 238 ℃, the reaction pressure is 50kPa, the residence time is 2 hours, the rotation speed of a stirrer is 100rpm, and an esterified melt is obtained after the reaction is finished;
after the titanium catalyst and fresh BDO are prepared, the titanium catalyst enters the esterification kettle 1 through a catalyst adding port in a spraying mode, wherein the spraying speed is 20m/s;
(b) Adding the esterified melt into a pre-shrinking kettle 2 from an outer chamber to perform pre-shrinking reaction, wherein the reaction conditions are as follows: the reaction temperature is 245 ℃, the reaction pressure is 2.0kPa, the residence time is 1.5 hours, the rotation speed of a stirrer is 60rpm, and the pre-polycondensed melt is obtained after the reaction is finished;
(c) The pre-polycondensation melt is produced from the inner chamber of the pre-polycondensation kettle 2 and is added into the final polycondensation kettle 3, and after the pre-polycondensation melt is thickened by the common baffle plates 31 and the heating baffle plates 32 which are alternately arranged at the inlet end of the final polycondensation kettle 3, the final polycondensation reaction is carried out under the following reaction conditions: the reaction temperature is 250 ℃, the reaction pressure is 80kPa, the residence time is 1h, the rotation speed of a stirrer is 9.0rpm, and the final polycondensation melt is obtained after the reaction is finished, namely the polybutylene terephthalate.
Comparative example 1: the difference from example 1 is that this comparative example uses an esterification tank stirrer speed of 100rpm, a final shrinkage tank stirrer speed of 7.5rpm, and the catalyst is added by spraying into the esterification tank from a catalyst addition port. The actual polymerization degree of the products of examples 1, 2, 3 and comparative example 1 described in the present invention are shown in Table 1.
TABLE 1 production parameters and degree of polymerization of the products
Claims (10)
1. An apparatus for preparing polybutylene terephthalate, comprising: esterification kettle (1), preshrinking cauldron (2) and final cauldron (3), its characterized in that, ordinary baffle (31) and heating baffle (32) of alternate arrangement are installed to the entry end of final cauldron (3), the middle part of ordinary baffle (31) is equipped with weir plate (33).
2. The device according to claim 1, characterized in that the height of the common baffle (31) is 1.2-3.0 times the height of the heating baffle (32).
3. The device according to claim 1, characterized in that the spacing of the common baffles (31) and the heating baffles (32) is proportional to the height of the common baffles (31).
4. An apparatus according to claim 1, characterized in that the height of the slice (33) decreases from the inlet end towards the inside.
5. The device according to claim 1, characterized in that the middle part of the heating baffle (32) is provided with a channel (34) and the inside is provided with a baffle plate (35) and a high-temperature heating medium.
6. A method of making a PBAT using the apparatus of claim 1, comprising the steps of:
(a) Adding mixed slurry of terephthalic acid and 1, 4-butanediol into an esterification kettle (1) for esterification reaction, and allowing a catalyst to enter the esterification kettle in a spraying manner through a catalyst adding port to react to obtain an esterification melt with an average polymerization degree of 5-20;
(b) Adding the esterified melt into a pre-shrinking kettle (2) for pre-shrinking polymerization reaction to obtain pre-shrinking melt with the average polymerization degree of 30-60;
(c) Adding the pre-condensed melt into a final condensation kettle (3), tackifying the pre-condensed melt at the inlet end of the final condensation kettle (3) through common baffles (31) and heating baffles (32) which are alternately arranged, and then carrying out final polycondensation reaction to obtain the final condensed melt with the average polymerization degree of 130-200, thus obtaining the polybutylene terephthalate.
7. The process of claim 6 wherein in step (a) the molar ratio of terephthalic acid to 1, 4-butanediol is from 1:2.0 to 1:3.2.
8. The process of claim 6 wherein in step (a) the catalyst is formulated with fresh BDO before being sprayed into the esterification kettle through a catalyst addition port.
9. The method according to claim 6, wherein the injection velocity of the catalyst is 10-30m/s.
10. The process of claim 7, wherein in steps (a) to (c), the esterification reaction conditions are: the reaction temperature is 236-246 ℃, the reaction pressure is 35-55kPa, the residence time is 1.5-3.5h, the rotation speed of the stirrer is 90-160rpm, and the conditions of the pre-polycondensation reaction are as follows: the reaction temperature is 245-255 ℃, the reaction pressure is 1.0-3.0kPa, the residence time is 1.5-3.0h, the rotation speed of a stirrer is 40-80rpm, and the conditions of the final polycondensation reaction are as follows: the reaction temperature is 245-255 ℃, the reaction pressure is 40-150kPa, the residence time is 0.8-2.0h, and the rotation speed of the stirrer is 2-10rpm.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210819918 | 2022-07-13 | ||
| CN2022108199183 | 2022-07-13 | ||
| CN2022114637912 | 2022-11-22 | ||
| CN202211463791 | 2022-11-22 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117398954A true CN117398954A (en) | 2024-01-16 |
Family
ID=89489612
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211508569.XA Pending CN117398954A (en) | 2022-07-13 | 2022-11-28 | Device and method for preparing polybutylene terephthalate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117398954A (en) |
-
2022
- 2022-11-28 CN CN202211508569.XA patent/CN117398954A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100487027C (en) | Polybutylene terephthalate pellet, compounded product thereof, molded product thereof and method for producing them | |
| CN1237091C (en) | Preparation method of poly-p-dioctyl phthalate butanediol ester and its manufacturing device | |
| JP3476833B2 (en) | Process for producing a copolyester of terephthalic acid, ethylene glycol and 1,4-cyclohexanedimethanol, exhibiting a neutral hue, high transparency and increased brightness | |
| JP4578752B2 (en) | Continuous process for producing poly (trimethylene terephthalate) | |
| CN107936237B (en) | Bio-based degradable polyester fiber and preparation method thereof | |
| CN107567470B (en) | Continuous process for preparing polybutylene terephthalate using purified terephthalic acid and 1, 4-butanediol | |
| CN1938361B (en) | Polybutylene terephthalate | |
| CN109456469B (en) | Preparation method of high-fluidity cation modified copolyester | |
| CN107915833B (en) | Fiber-grade bio-based polyester and preparation method thereof | |
| CN109134834B (en) | Preparation method of isosorbide copolyester | |
| CN111394831B (en) | Method for preparing polyester-nylon composite fiber through melt direct spinning | |
| CN111423570B (en) | Process and device for continuously producing degradable polyester | |
| CN100424114C (en) | Method for producing polybutylene terephthalate | |
| CN109485838B (en) | Copolymerization type high-fluidity cationic polyester master batch matrix material and preparation method thereof | |
| CN1487964A (en) | Process for manufacture of polyesters based on 1,4-cyclohexanedimethanol and isophthalicacid | |
| CN109180923B (en) | High-fluidity stain-resistant easy-to-dye polyester master batch and preparation method thereof | |
| CN117398954A (en) | Device and method for preparing polybutylene terephthalate | |
| CN101855268A (en) | Method for producing poly(trimethylene terephthalate) | |
| CN108892770B (en) | Method for inhibiting side reaction of tetrahydrofuran in polymerization process | |
| CN111116882B (en) | Full-biodegradable copolyester and preparation method and application thereof | |
| CN111101227B (en) | Full-biodegradable copolyester fiber and preparation method thereof | |
| CN111116883B (en) | Biodegradable copolyester and preparation method thereof | |
| CN108774312B (en) | Low-viscosity polyester and preparation method thereof | |
| CN102060983B (en) | Preparation method of cyclic polyester oligomer | |
| CN109456468B (en) | Copolymerization type high-fluidity hydrophilic easy-dyeing polyester master batch matrix material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |