CN110790907A - Production equipment and process flow of full-continuous PETG - Google Patents
Production equipment and process flow of full-continuous PETG Download PDFInfo
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- CN110790907A CN110790907A CN201911130256.3A CN201911130256A CN110790907A CN 110790907 A CN110790907 A CN 110790907A CN 201911130256 A CN201911130256 A CN 201911130256A CN 110790907 A CN110790907 A CN 110790907A
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- reaction kettle
- esterification
- kettle
- polycondensation
- reaction
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 229920005644 polyethylene terephthalate glycol copolymer Polymers 0.000 title claims description 17
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 72
- 238000005886 esterification reaction Methods 0.000 claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 29
- 238000005507 spraying Methods 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- 230000032050 esterification Effects 0.000 claims abstract description 20
- 238000004537 pulping Methods 0.000 claims abstract description 16
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 38
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000155 melt Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 6
- 239000012071 phase Substances 0.000 claims 3
- 239000007792 gaseous phase Substances 0.000 claims 2
- 239000002002 slurry Substances 0.000 abstract description 8
- 238000005520 cutting process Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000010009 beating Methods 0.000 description 4
- -1 polyethylene terephthalate Polymers 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005453 pelletization Methods 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920006300 shrink film Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229920001634 Copolyester Polymers 0.000 description 1
- 101100299498 Xenopus laevis pteg gene Proteins 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000071 blow moulding Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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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
-
- 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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention provides production equipment of full-continuous modified PETG, which comprises an NPG preparation kettle, a batching and pulping kettle, an esterification first reaction kettle, an esterification second reaction kettle, a process tower, a first pre-polycondensation reaction kettle, a first pre-polymerization spraying system, a second pre-polycondensation reaction kettle, a second pre-polymerization spraying system, a final polycondensation reaction kettle, a final polymerization spraying system, a pre-polymerization and final polymerization vacuum system and a particle cutting system. The slurry proportioning and pulping kettle is connected with the first esterification reaction kettle, the first esterification reaction kettle is connected with the second esterification reaction kettle, the first esterification reaction kettle and the second esterification reaction kettle are connected with the process tower in a gas phase mode, the second esterification reaction kettle is connected with the first pre-polycondensation reaction kettle, the bottom of the first pre-polycondensation reaction kettle is connected with the bottom of the second pre-polycondensation front end, and the bottom of the second pre-polycondensation reaction kettle is connected with the bottom of the final polycondensation reaction kettle front end.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to production equipment and a process flow of full-continuous PETG.
Background
PETG is a non-crystalline copolyester. Since a certain amount of ethylene glycol is substituted by neopentyl glycol (NPG) during the production thereof, crystallization can be prevented, thereby improving the manufacturing process and transparency. The product is highly transparent, has excellent shock resistance, is particularly suitable for forming thick-wall transparent products, has excellent processing and forming performance, can be designed into any shape according to the intention of a designer, can be widely applied to the markets of plates, sheets, high-performance shrink films, bottles, profiles and the like by adopting traditional forming methods such as extrusion, injection molding, blow molding, plastic suction and the like, has excellent secondary processing performance and can be subjected to conventional machining decoration. The polyethylene terephthalate glycol neopentyl glycol ester (PETG) has high transparency, excellent impact resistance and good thermoplastic property, is widely used for sheet materials, and is a high-performance shrink film, excellent in comprehensive performance, high in cost performance and good in market prospect.
Disclosure of Invention
The invention aims to achieve the aim and provides the production equipment and the process flow of the full-continuous PETG, which have the advantages of reasonable process, high automation degree, high production efficiency, stable product quality and safe and stable operation.
The purpose of the invention is realized as follows:
a production device and a process flow of a full-continuous PETG (polyethylene terephthalate glycol), which comprises a pulping system for carrying NPG, EG and PTA materials for mixing and pulping, and further comprises an esterification reaction system for carrying out esterification reaction on the mixed pulp, a polycondensation reaction system for carrying out pre-polycondensation and final polycondensation reaction on the finished raw materials, and a grain cutting system for melting and cutting grains on the raw materials subjected to pre-polycondensation and final polycondensation, and is characterized in that the pulping system comprises a preliminary pulp preparation tank, a buffer tank, an NPG (polyethylene terephthalate glycol) preparation kettle and a batching and pulping kettle, wherein the bottom of the preliminary pulp preparation tank is connected with the top of the buffer tank through a pipeline, the buffer tank is connected with the top of the NPG preparation kettle through a pipeline, and the bottom of the NPG preparation kettle is connected with the batching and pulping kettle through a pipeline;
the esterification reaction system comprises an esterification first reaction kettle, an esterification second reaction kettle and a process tower, the esterification reaction system is connected with the pulping system through a screw pump, the esterification first reaction kettle is connected with the esterification second reaction kettle through a pipeline, the esterification first reaction kettle and the esterification second reaction kettle are connected with the lower part of the process tower through pipeline gas phases, and process tower recycled liquid forms reflux with the esterification first reaction kettle and the esterification second reaction kettle;
the polycondensation reaction system comprises a pre-polycondensation reaction kettle, a first pre-polymerization spraying system, a second pre-polycondensation reaction kettle, a second pre-polymerization spraying system, a final polycondensation reaction kettle, a final polycondensation spraying system, a pre-polymerization and final polycondensation vacuum system, the polycondensation reaction system is arranged in the esterification reaction system, the first pre-polycondensation reaction kettle is connected with the second esterification reaction kettle through a pipeline, gas generated by the first pre-polycondensation reaction kettle is conveyed into the first pre-polymerization spraying system through a pipeline gas phase, the bottom of the first pre-polycondensation reaction kettle is connected with the bottom of the second pre-polycondensation front end, gas generated by the second pre-polycondensation reaction kettle is conveyed into the second pre-polymerization spraying system through a pipeline gas phase, the bottom of the second pre-polycondensation reaction kettle is connected with the bottom of the final polycondensation reaction kettle through a pipeline gas phase, and the gas generated by the final polycondensation reaction kettle is conveyed into the final polycondensation spraying system through a pipeline gas phase, the gas phases of the first pre-polymerization spraying system, the second pre-polymerization spraying system and the final polymerization spraying system are all connected with a pre-polymerization and final polymerization vacuum system; the melt produced by the final polycondensation reaction kettle enters a granulating system for granulation through pressurization;
furthermore, according to the requirements of different manufacturers, the NPG preparation kettle adopts intermittent preparation, and the feeding amounts of Ethylene Glycol (EG) and neopentyl glycol (NPG) are controlled according to a certain proportion;
further, feeding a catalyst of an esterification reaction kettle into the reaction kettle in a manner of diluting a mixed solution of the top and a refluxing process tower recovery liquid;
furthermore, the final polycondensation reaction kettle is a single-end-shaft disk vacuum reactor, a plurality of film-forming disks are arranged on the stirring shaft to form a two-disk stirring system, and the viscosity of the PETG product can meet higher requirements.
Compared with the prior art, the invention has the beneficial effects that:
the invention has the advantages of compact structure, reasonable process, high automation degree, high production efficiency, stable product quality and safe and stable operation. Through the mixing of EG and NPG, the slurry preparation is better carried out; the second pre-shrinking kettle adopts higher vacuum reaction to ensure the overflow of more micromolecules, thereby ensuring that the viscosity of the PETG product can meet higher requirements; and the underwater bracing and granulating mode is adopted, so that the forming of the sliced particles is ensured.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
1. A preliminary slurry preparation tank; 2. a buffer tank; 3. NPG preparation kettle; 4. a material blending and pulping kettle; 5, esterifying a reaction kettle; 6. esterification reaction kettle II; 7. a process tower; 8. a first pre-polycondensation reaction kettle; 9. a first pre-polymerization spray system; 10. a second pre-polycondensation reaction kettle; 11. a second pre-polymerization spraying system; 12. a final polycondensation reaction kettle; 13. a final focusing spray system; 14. a prepolymerization and final polymerization vacuum system; 15. and a pelletizing system.
Detailed Description
As shown in figure 1, the production equipment and the process flow of the full-continuous PETG as shown in figure 1 and the batching and beating system in the process flow comprise a primary slurry preparation tank 1, a buffer tank 2, an NPG preparation kettle 3 and a batching and beating kettle 4, wherein PTA and EG enter the buffer tank 2 after the primary slurry preparation tank 1 is prepared, are buffered and then are sent into the NPG preparation kettle 3 to be prepared according to the proportion and then are sent into the batching and beating kettle 4, and the slurry after beating is sent into an esterification reaction system through a screw pump.
As shown in figure 1, the esterification reaction kettle system in the production equipment and the process flow of the fully continuous PTEG comprises an esterification first reaction kettle 5, an esterification second reaction kettle 6 and a process tower 7. And (2) feeding the slurry from the blending and pulping kettle 4 into an esterification reaction kettle 5 for esterification reaction, controlling the reaction temperature to be 190-250 ℃ and the reaction pressure to be 80KPa (A), mixing a catalyst agent with the recovery liquid, adding the mixture into the reaction kettle for reaction, feeding the mixture into an esterification reaction kettle 6 after the reaction is finished, controlling the reaction temperature to be 190-250 ℃ and the reaction pressure to be 5KPa (A), mixing an additive with the recovery liquid, adding the mixture into the reaction kettle for continuous reaction, and controlling and conveying the esterified product to a first pre-polycondensation reaction kettle 8 through an adjusting valve. The process gas generated by the esterification reaction and the like are separated and recovered from the process tower 7 through a gas phase pipeline;
as shown in figure 1, the production equipment, the process flow and the polycondensation reaction kettle system and the pelletizing system in the process flow of the fully continuous PETG comprise a first pre-polycondensation reaction kettle 8, a first pre-polymerization spraying system 9, a second pre-polycondensation reaction kettle 10, a second pre-polymerization spraying system 11, a final polycondensation reaction kettle 12, a final polymerization spraying system 13, a pre-polymerization and final polymerization vacuum system 14 and a pelletizing system 15. After the esterified substance enters a first pre-polycondensation reaction kettle 8, a pre-polycondensation reaction is carried out, the temperature of the first pre-polycondensation reaction kettle 8 is controlled to be 260-270 ℃, the reaction pressure is 2-5 KPa (A), then the esterified substance enters a second pre-polycondensation reaction kettle 10 through an adjusting valve under the potential difference and the pressure difference for reaction, the temperature is controlled to be 265-275 ℃, the reaction pressure is 0.8-1 KPa (A), and the reacted prepolymer enters a final polycondensation reaction kettle 12. And the generated gas phase component water, EG and the like enter a corresponding prepolymerization spraying system. And (3) after the prepolymer enters a final polycondensation reaction kettle 12, carrying out final polycondensation reaction, wherein the reaction temperature is controlled to be 270-275 ℃, and the reaction pressure is 90-110 Pa (A). The melt after reaction has high viscosity, and is conveyed to a melt filter through a melt pump, filtered and then conveyed to a granulator for granulation. Gas-phase components generated in the final polycondensation reaction are recovered through a final polycondensation spraying system 13, and the vacuum of the final polycondensation reaction kettle and the spraying system is provided by a prepolymerization and final polycondensation vacuum system 14.
The invention has the advantages of compact structure, reasonable process, high automation degree, high production efficiency, stable product quality and safe and stable operation. Through the mixing of EG and NPG, the slurry preparation is better carried out; the second pre-shrinking kettle adopts higher vacuum reaction to ensure the overflow of more micromolecules, thereby ensuring that the viscosity of the PETG product can meet higher requirements; and the underwater bracing and granulating mode is adopted, so that the forming of the sliced particles is ensured.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (4)
1. The production equipment and the process flow of the full-continuous PETG comprise a pulping system for carrying NPG, EG and PTA materials for mixing and pulping, and further comprise an esterification reaction system for carrying out esterification reaction on the mixed pulp, a polycondensation reaction system for carrying out pre-polycondensation and final polycondensation reaction on the finished raw materials, and a granulating system for granulating the pre-polycondensation and final polycondensation finished raw materials, and are characterized in that the pulping system comprises a preliminary pulp preparation tank (1), a buffer tank (2), an NPG preparation kettle (3) and a batching pulping kettle (4), wherein the bottom of the preliminary pulp preparation tank (1) is connected with the top of the buffer tank (2) through a pipeline, the buffer tank (2) is connected with the top of the NPG preparation kettle (3) through a pipeline, and the bottom of the NPG preparation kettle (3) is connected with the batching pulping kettle (4) through a pipeline.
The esterification reaction system comprises an esterification first reaction kettle (5), an esterification second reaction kettle (6) and a process tower (7), the esterification reaction system is connected with a pulping system through a screw pump, the esterification first reaction kettle (5) is connected with the esterification second reaction kettle (6) through a pipeline, the esterification first reaction kettle (5) and the esterification second reaction kettle (6) are both connected with the lower part of the process tower (7) through a pipeline gas phase, and a recovery liquid of the process tower (7) forms reflux with the esterification first reaction kettle (5) and the esterification second reaction kettle (6);
polycondensation reaction system includes a pre-polycondensation reaction cauldron (8), first prepolymerization spray system (9), second pre-polycondensation reaction cauldron (10), second prepolymerization spray system (11), final polycondensation reaction cauldron (12), final polycondensation spray system (13), prepolymerization and final polycondensation vacuum system (14), polycondensation reaction system arranges on esterification reaction system right side, first pre-polycondensation reaction cauldron (8) link to each other with esterification reaction cauldron (6) through the pipeline, the gas that first pre-polycondensation reaction cauldron (8) produced is carried in first prepolymerization spray system (9) through pipeline gaseous phase, first pre-polycondensation reaction cauldron (8) bottom links to each other with second pre-polycondensation (10) front end bottom through the pipeline, the gas that second pre-polycondensation reaction cauldron (10) produced is carried in second prepolymerization spray system (11) through pipeline gaseous phase, second pre-polycondensation reaction cauldron (10) bottom is carried in pipeline and final polycondensation reaction cauldron (12) front end bottom through the pipeline The gas generated by the final polycondensation reaction kettle (12) is conveyed into a final polymerization spraying system (13) through a pipeline gas phase, and the first pre-polymerization spraying system (9), the second pre-polymerization spraying system (11) and the final polymerization spraying system are all connected with a pre-polymerization and final polymerization vacuum system (14) through the pipeline gas phase (13); and the melt produced by the final polycondensation reaction kettle (12) enters a granulating system for granulation through pressurization.
2. The equipment and process for producing full-continuous PETG as claimed in claim 1, wherein the NPG preparation kettle (3) is intermittently prepared, and the feeding amounts of Ethylene Glycol (EG) and neopentyl glycol (NPG) are controlled according to the requirements of different manufacturers and a certain ratio.
3. The equipment and process for producing full-continuous PETG according to claim 1, characterized in that the catalyst feed of the esterification reaction kettle (5) is added into the reaction kettle by diluting the mixed solution of the top and the recycled solution of the reflux process tower (7).
4. The production equipment and the process flow of the fully continuous PETG according to the claim 1 are characterized in that the final polycondensation reaction kettle (12) is a single-end-shaft disc vacuum reactor, a stirring shaft is provided with a plurality of film-forming discs to form a two-disc stirring system, and the viscosity of the PETG product can meet higher requirements.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911130256.3A CN110790907A (en) | 2019-11-18 | 2019-11-18 | Production equipment and process flow of full-continuous PETG |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911130256.3A CN110790907A (en) | 2019-11-18 | 2019-11-18 | Production equipment and process flow of full-continuous PETG |
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| Publication Number | Publication Date |
|---|---|
| CN110790907A true CN110790907A (en) | 2020-02-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911130256.3A Pending CN110790907A (en) | 2019-11-18 | 2019-11-18 | Production equipment and process flow of full-continuous PETG |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724388A (en) * | 2020-12-28 | 2021-04-30 | 扬州普立特科技发展有限公司 | Production device for recycling polyester to be regenerated into degradable material PBAT |
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| CN102691131A (en) * | 2012-06-19 | 2012-09-26 | 福建经纬新纤科技实业有限公司 | Manufacturing equipment system of flame-retardant polyester fiber |
| CN104710602A (en) * | 2015-03-05 | 2015-06-17 | 浙江万凯新材料有限公司 | Preparation method of copolymerization polymer |
| CN107892744A (en) * | 2017-11-24 | 2018-04-10 | 安徽皖维高新材料股份有限公司 | A kind of preparation method of Heat Shrinkage Film Polyester section |
| 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 |
-
2019
- 2019-11-18 CN CN201911130256.3A patent/CN110790907A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102691131A (en) * | 2012-06-19 | 2012-09-26 | 福建经纬新纤科技实业有限公司 | Manufacturing equipment system of flame-retardant polyester fiber |
| CN104710602A (en) * | 2015-03-05 | 2015-06-17 | 浙江万凯新材料有限公司 | Preparation method of copolymerization polymer |
| CN107892744A (en) * | 2017-11-24 | 2018-04-10 | 安徽皖维高新材料股份有限公司 | A kind of preparation method of Heat Shrinkage Film Polyester section |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724388A (en) * | 2020-12-28 | 2021-04-30 | 扬州普立特科技发展有限公司 | Production device for recycling polyester to be regenerated into degradable material PBAT |
| CN112724388B (en) * | 2020-12-28 | 2023-06-23 | 扬州普立特科技发展有限公司 | Production device for recycling polyester into degradable material PBAT |
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Application publication date: 20200214 |