CN117753338A - Polycondensation kettle device for regenerating DMT and copolyester thereof - Google Patents
Polycondensation kettle device for regenerating DMT and copolyester thereof Download PDFInfo
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- CN117753338A CN117753338A CN202311710387.5A CN202311710387A CN117753338A CN 117753338 A CN117753338 A CN 117753338A CN 202311710387 A CN202311710387 A CN 202311710387A CN 117753338 A CN117753338 A CN 117753338A
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- 229920001634 Copolyester Polymers 0.000 title claims abstract description 36
- 238000006068 polycondensation reaction Methods 0.000 title claims abstract description 30
- 230000001172 regenerating effect Effects 0.000 title claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 127
- 230000001105 regulatory effect Effects 0.000 claims abstract description 67
- 239000000463 material Substances 0.000 claims abstract description 44
- 230000000712 assembly Effects 0.000 claims abstract description 18
- 238000000429 assembly Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims description 57
- 238000000034 method Methods 0.000 claims description 33
- 238000003860 storage Methods 0.000 claims description 28
- 230000007246 mechanism Effects 0.000 claims description 25
- 230000008569 process Effects 0.000 claims description 19
- 230000002093 peripheral effect Effects 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 abstract description 29
- 229920000728 polyester Polymers 0.000 abstract description 24
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 18
- 239000002699 waste material Substances 0.000 abstract description 16
- 238000000265 homogenisation Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 5
- 230000008859 change Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 35
- 238000006136 alcoholysis reaction Methods 0.000 description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 238000005809 transesterification reaction Methods 0.000 description 19
- 239000003054 catalyst Substances 0.000 description 12
- 230000035484 reaction time Effects 0.000 description 12
- 230000009477 glass transition Effects 0.000 description 8
- 238000002844 melting Methods 0.000 description 8
- 230000008018 melting Effects 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 150000002148 esters Chemical group 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- LLLVZDVNHNWSDS-UHFFFAOYSA-N 4-methylidene-3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound C1(C2=CC=C(C(=O)OC(=C)O1)C=C2)=O LLLVZDVNHNWSDS-UHFFFAOYSA-N 0.000 description 1
- 240000005523 Peganum harmala Species 0.000 description 1
- -1 Polyethylene terephthalate Polymers 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
- C08J11/22—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds
- C08J11/24—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic oxygen-containing compounds containing hydroxyl groups
-
- 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
-
- 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
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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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)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Polyesters Or Polycarbonates (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
Abstract
The invention discloses a polycondensation kettle device for regenerating DMT and copolyester thereof, which belongs to the field of waste polyester recycling, and comprises a kettle body, and a rotating shaft which is vertical in the up-down direction in the kettle body and is driven to rotate by a motor; two groups of stirring assemblies are arranged on a rotating shaft in the kettle body, each stirring assembly comprises a rotating seat, a plurality of stirring rods and paddles, the rotating seats are fixedly arranged on the rotating shaft, and the stirring rods and the paddles correspond to each other one by one; the blade inclination angles of the two groups of stirring assemblies are opposite, the stirring assembly on the upper side can push materials downwards, and the stirring assembly on the upper side can push materials upwards. According to the invention, by adopting the reaction kettle device, the raw materials in the copolyester production process can be subjected to homogenization mixing treatment, the mixing rate of each material is regulated according to the temperature change condition in the mixing reaction process, the heating and mixing homogenization degree of the materials in the mixing reaction process are maintained, and the efficient and stable mixing effect is achieved.
Description
Technical Field
The invention relates to the field of recycling of waste polyesters, in particular to a polycondensation kettle device for regenerating DMT and copolyester thereof.
Background
Polyethylene terephthalate (PET, commonly known as polyester) is widely used as an important raw material for the production of beverage bottles, fibers, films, sheets, and the like. With the rapid development of the polyester industry, the polyester waste generated during the production of polyester and the processing and use of products is also rapidly growing. Because polyester has strong chemical inertness, the polyester is difficult to degrade or decompose by microorganisms in natural storage, so that huge resource waste is caused, and serious environmental pollution is generated. Therefore, recycling is an important issue in the current polyester industry to realize recycling of resources and improve environmental quality.
At present, the waste polyester is recycled mainly by a physical method and a chemical method. The physical method is mainly to prepare the waste polyester and the products thereof into regenerated slices through simple physical processes such as direct blending, granulating and the like, and then to use the regenerated slices, but the method is mainly applicable to recycling waste polyester with single components such as polyester waste bottles, waste filaments and the like, and the spinnability and the fiber quality of spinning are affected due to large quality fluctuation of the regenerated slices. The chemical method mainly comprises a hydrolysis method, a methanol alcoholysis method, an ethylene glycol alcoholysis method and the like, but the hydrolysis method and the methanol alcoholysis method have the defects of harsh reaction conditions, low recovery efficiency and the like. The general reaction temperature of the glycol alcoholysis method is 180-250 ℃ and the pressure is 0.1-0.6 MPa, and compared with the hydrolysis method and the methanol alcoholysis method, the reaction condition is mild and the reaction safety is good. However, the alcoholysis product obtained by alcoholysis of ethylene glycol is ethylene terephthalate (BHET), the purification process is complex, and for this purpose, a regeneration process of alcoholysis of ethylene glycol and transesterification of methanol is developed by Japanese Di company, which makes a major breakthrough in recovering waste polyester by chemical method, but the regenerated polyester by chemical method is mainly conventional polyester at present.
Disclosure of Invention
The invention aims to solve the problems and provide a polycondensation kettle device for regenerating DMT and copolyester thereof, which can improve the uniformity of internal materials in the reaction process and is beneficial to the production of final copolyester products.
The invention provides a polycondensation kettle device for regenerating DMT and copolyester thereof, which comprises a kettle body, wherein a rotating shaft is vertically arranged in the kettle body, and the rotating shaft is driven to rotate by a motor; two groups of stirring assemblies are arranged on a rotating shaft in the kettle body, each stirring assembly comprises a rotating seat, a plurality of stirring rods and paddles, the rotating seats are fixedly arranged on the rotating shaft, the stirring rods and the paddles correspond to each other one by one, the stirring rods and the paddles are two groups, and the stirring rods and the paddles are arranged on the periphery of the rotating seat and are distributed in an annular circumference array manner;
the blade angles of the two groups of stirring assemblies are opposite, the stirring assembly on the upper side can push materials downwards, and the stirring assembly on the upper side can push materials upwards;
the stirring assembly further comprises an adjusting mechanism, wherein the adjusting mechanism is arranged at the peripheral position of the rotating shaft and is linked with the rotating seat, so that the inclination angle of the blade can be adjusted; the adjusting mechanism comprises an adjusting sleeve and a plurality of hinging rods, and the adjusting sleeve is sleeved outside the rotating shaft and can axially slide along the rotating shaft for adjustment; the number of the hinging rods corresponds to that of the stirring rods one by one, and the positions between the adjusting sleeves can be realized through the hinging rods; the periphery of the stirring rod is fixedly connected with a first hinge seat, the periphery of the stirring rod is fixedly connected with a second hinge seat, two ends of the hinge rod are respectively hinged between the first hinge seat and the second hinge seat, and linkage between the adjusting sleeve and the stirring rod is realized through the hinge rod; in the up-down sliding adjusting process, the adjusting sleeve can drive the stirring rod to swing and adjust, and then the inclination angle of the blade can be adjusted.
The invention is further characterized in that an adjusting ring is sleeved on the periphery of the adjusting sleeve, the adjusting ring is rotationally connected with the adjusting sleeve and mutually axially limited, and the adjusting sleeve is adjusted up and down through the adjusting ring.
The invention is further characterized in that a lifting sleeve is externally sleeved at the middle section of the rotating shaft, a supporting sleeve is sleeved at the periphery of the lifting sleeve, the supporting sleeve is fixedly arranged at the center position in the kettle body, and the periphery of the supporting sleeve is supported and fixed through a supporting rod; the upper end and the lower end of the lifting sleeve penetrate through the supporting sleeve and are fixedly connected with the adjusting rings of the upper stirring assembly and the lower stirring assembly respectively; the lifting sleeve drives the blade inclination angles in the two groups of adjusting mechanisms to adjust in the lifting process.
The invention is further arranged that the upper end and the lower end of the supporting sleeve are respectively provided with a through hole for the lifting sleeve to penetrate, and the through holes and the lifting sleeve are sealed by a sliding sealing piece; the outer periphery of the lifting sleeve is fixedly connected with a lifting piston, the lifting piston is positioned in the supporting sleeve and is positioned in the relative middle position of the lifting sleeve, and a piston connecting structure is formed between the lifting piston and the inner periphery of the supporting sleeve; the lifting piston forms a sealed state, sliding sealing pieces are arranged at the through holes at the upper end and the lower end, and a sealed cavity is formed at the inner peripheral position of the supporting sleeve.
The invention is further arranged that the lifting piston respectively comprises an upper cavity and a lower cavity of the inner cavity of the lifting sleeve, one side is a pressure regulating cavity, the other side is a spring cavity, the regulating cavity is filled with thermal expansion liquid, the other side is provided with a spring, and the two sides of the lifting piston respectively play a supporting role; in the heating process, the thermal expansion liquid generates thermal expansion to push the lifting piston to drive the lifting sleeve and the adjusting mechanism to act.
The invention is further provided that the pressure regulating cavity can be positioned at the upper side of the spring cavity, and the lifting piston realizes up-down balance through the pressure of the thermal expansion liquid and the elasticity of the spring; when the temperature of the inner cavity of the kettle body is increased, the thermal expansion liquid is heated and expanded, the lifting piston is pushed to overcome the spring pressure to move, the lifting sleeve and the adjusting mechanism are driven to act, the inclination angle of the blade in the stirring assembly is increased, and the stirring efficiency of the stirring assembly is improved; when the temperature of the inner cavity of the kettle body is reduced, the thermal expansion liquid contracts, the spring pushes the lifting piston to move, the lifting sleeve and the adjusting mechanism are driven to act, the inclination angle of the blade in the stirring assembly is reduced, and the stirring efficiency of the stirring assembly is reduced.
The invention is further arranged that the supporting rod is fixedly connected to the periphery of the supporting sleeve and is positioned at one side of the thermal expansion liquid, a runner communicated with the inner cavity of the supporting sleeve is arranged in the supporting rod, the runner is communicated with the pressure regulating cavity in the supporting sleeve, and the thermal expansion cavity in the supporting sleeve can be communicated with the external pressure regulating device through the runner.
The invention is further provided that a heating device is arranged in the kettle body, and the heating device is arranged in the side wall of the kettle body; a liquid storage box is fixedly arranged at the inner peripheral position of the side wall of the kettle body, the liquid storage box is of a closed cavity structure, and the inside of the liquid storage box is filled with thermal expansion liquid; the liquid storage box is fixedly connected with the support rod, a flow passage is arranged in the support rod, and the pressure regulating cavity is communicated with the liquid storage box through the flow passage.
The invention is further provided that the outer side of the liquid storage box is connected with a conduit, the conduit penetrates through the side wall of the kettle body and extends out of the kettle body, a second electromagnetic valve is arranged on the conduit, and the conduit is connected to an external pressure regulating device.
According to the invention, by adopting the reaction kettle device, the raw materials in the copolyester production process can be subjected to homogenization mixing treatment, the mixing rate of each material is regulated according to the temperature change condition in the mixing reaction process, the heating and mixing homogenization degree of the materials in the mixing reaction process are maintained, and the efficient and stable mixing effect is achieved.
Drawings
FIG. 1 is a schematic view of a polycondensation reaction vessel in the present invention;
FIG. 2 is an enlarged view of a portion of the present invention;
FIG. 3 is a schematic view showing the structure of the inside of a supporting rod in the polycondensation reaction vessel of the present invention;
fig. 4 is a schematic structural view of the stirring assembly of the present invention.
Reference numerals: 1. a kettle body; 2. a rotating shaft; 3. a motor; 4. a stirring assembly; 5. a support sleeve; 6. a support rod; 7. a lifting sleeve; 8. a lifting piston; 9. a pressure regulating cavity; 10. a spring cavity; 11. a through hole; 12. a flow passage; 13. a first electromagnetic valve; 14. a liquid storage box; 15. a liquid storage cavity; 16. a balancing cavity; 17. a balance piston; 18. a conduit; 19. a second electromagnetic valve; 20. a pressure regulating device; 21. a sidewall; 22. a heating device; 23. a connecting frame; 41. a rotating seat; 42. a stirring rod; 43. a paddle; 44. an adjusting sleeve; 45. a hinge seat I; 46. a hinge seat II; 47. a hinge rod; 48. a limit convex ring; 49. a limit ring groove; 410. an adjusting ring.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
All physical property indexes of the regenerated copolyester chips are executed according to a GBT 14190-2008 fiber grade polyester chip (PET) test method.
Example 1:
the embodiment discloses a preparation method of regenerated DMT and copolyester thereof, which comprises the following steps:
the pretreated waste polyester is put into an alcoholysis kettle according to the mass ratio of the waste polyester to the glycol of 1:2, and the addition amount of the alcoholysis catalyst is 2 per mill. Controlling the reaction temperature to 190 ℃ and the reaction time to 4 hours to obtain an alcoholysis product containing BHET, and filtering the alcoholysis product and sending the alcoholysis product into an ester exchange kettle.
Controlling the transesterification reaction temperature to 60 ℃ and the reaction time to 4 hours, adding BHET: methanol with the molar ratio of 1:2 is added with 0.2 per mill of transesterification catalyst, and the obtained transesterification product is filtered, centrifuged, distilled and the like to obtain refined DMT with the purity of more than 99.9 percent.
CHDM 5% (mole percent with DMT) and excess Ethylene Glycol (EG) were added to control total alcohol: DMT molar ratio is 2:1, 0.2 per mill of transesterification catalyst is added, the temperature of the transesterification reaction is controlled to be 190 ℃, and the reaction time is 4 hours. The obtained transesterification liquid enters a pre-polycondensation kettle.
The temperature of the polycondensation-I and the polycondensation-II are controlled to be 220 ℃ and 240 ℃ respectively, the absolute pressure is 1-100 KPa, 0.4 permillage stabilizer, 0.2 permillage polycondensation catalyst and 0.5 permillage antioxidant are added, and the intrinsic viscosity of the prepolymer is 0.30dL/g. Then the mixture enters a vertical final polycondensation kettle, the reaction temperature is controlled at 260 ℃, the absolute pressure is controlled at 0.1-1 KPa, the reaction time is 2.0h, and then the mixture is discharged through a booster pump, filtered, granulated and packaged. The intrinsic viscosity of the finally obtained recycled copolyester was 0.780dL/g, the melting point was 228 ℃, the glass transition temperature was 85 ℃ and the b value was 5.8 (the results are shown in Table 1).
Example 2:
the embodiment discloses a preparation method of regenerated DMT and copolyester thereof, which comprises the following steps:
the pretreated waste polyester is put into an alcoholysis kettle according to the mass ratio of the waste polyester to the glycol of 1:2.5, and the addition amount of the alcoholysis catalyst is 2 per mill. Controlling the reaction temperature to 200 ℃ and the reaction time to 3 hours to obtain an alcoholysis product containing BHET, and filtering the alcoholysis product and sending the alcoholysis product into an ester exchange kettle.
Controlling the transesterification reaction temperature to 65 ℃ and the reaction time to 3.5h, adding BHET: methanol with the molar ratio of 1:2.5 is added with 0.2 per mill of transesterification catalyst, and the obtained transesterification product is filtered, centrifuged, distilled and the like to obtain refined DMT with the purity of more than 99.9 percent.
10% (mole percent with DMT) of CBDO and excess Ethylene Glycol (EG) were added to control total alcohol: DMT molar ratio is 2.5:1, 0.2 per mill of transesterification catalyst is added, the temperature of transesterification reaction is controlled to be 200 ℃, and the reaction time is 3 hours. The obtained transesterification liquid enters a pre-polycondensation kettle.
The temperature of the polycondensation-I and the polycondensation-II are controlled to be 230 ℃ and 250 ℃ respectively, the absolute pressure is 1-100 KPa, 0.4 permillage stabilizer, 0.2 permillage polycondensation catalyst and 0.5 permillage antioxidant are added, and the intrinsic viscosity of the prepolymer is 0.35dL/g. Then the mixture enters a vertical final polycondensation kettle, the reaction temperature is controlled to be 270 ℃, the absolute pressure is controlled to be 0.1-1 KPa, the reaction time is 1.5h, and then the mixture is discharged through a booster pump, filtered, granulated and packaged. The intrinsic viscosity of the finally obtained recycled copolyester was 0.720dL/g, the melting point was 215 ℃, the glass transition temperature was 92.5 ℃ and the b value was 6.1 (the results are shown in Table 1).
Example 3:
the embodiment discloses a preparation method of regenerated DMT and copolyester thereof, which comprises the following steps:
the pretreated waste polyester is put into an alcoholysis kettle according to the mass ratio of the waste polyester to the glycol of 1:3, and the addition amount of the alcoholysis catalyst is 2 per mill. Controlling the reaction temperature to 210 ℃ and the reaction time to 2 hours to obtain an alcoholysis product containing BHET, and filtering the alcoholysis product and sending the alcoholysis product into an ester exchange kettle.
Controlling the transesterification reaction temperature to 70 ℃ and the reaction time to 3 hours, and adding BHET: methanol with the molar ratio of 1:3 is added with 0.2 per mill of transesterification catalyst, and the obtained transesterification product is filtered, centrifuged, distilled and the like to obtain refined DMT with the purity of more than 99.9 percent.
15% (mole percent with DMT) of ISB and excess Ethylene Glycol (EG) were added to control total alcohol: DMT molar ratio is 3:1, 0.2 per mill of transesterification catalyst is added, the temperature of the transesterification reaction is controlled to be 210 ℃, and the reaction time is 2 hours. The obtained transesterification liquid enters a pre-polycondensation kettle.
The temperature of the polycondensation-I and the polycondensation-II are controlled to be 240 ℃ and 260 ℃ respectively, the absolute pressure is 1-100 KPa, 0.4 permillage stabilizer, 0.2 permillage polycondensation catalyst and 0.5 permillage antioxidant are added, and the intrinsic viscosity of the prepolymer is 0.40dL/g. Then enters a vertical final polycondensation kettle, the reaction temperature is controlled to be 280 ℃, the absolute pressure is controlled to be 0.1-1 KPa, the reaction time is 1.0h, and then the materials are discharged through a booster pump, filtered, granulated and packaged. The final regenerated copolyester had an intrinsic viscosity of 0.687dL/g, a melting point of 201℃and a glass transition temperature of 95℃and a b value of 6.5 (the results are shown in Table 1).
Example 4:
this example discloses a process for the preparation of regenerative DMT and its copolyesters, as described in example 2, with the difference that: 5% (mole percent with DMT) of CHDM and 5% (mole percent with DMT) of CBDO were added. The intrinsic viscosity of the finally obtained recycled copolyester was 0.685dL/g, the melting point was 211 ℃, the glass transition temperature was 96.8 ℃ and the b value was 6.7 (the results are shown in Table 1).
Example 5:
this example discloses a process for the preparation of regenerative DMT and its copolyesters, as described in example 2, with the difference that: 5% (mole percent with DMT) of CHDM and 5% (mole percent with DMT) of ISB were added. The intrinsic viscosity of the finally obtained recycled copolyester was 0.679dL/g, the melting point was 209 ℃, the glass transition temperature was 96℃and the b-value was 6.8 (the results are shown in Table 1).
Example 6:
this example discloses a process for the preparation of regenerative DMT and its copolyesters, as described in example 2, except that 5% (mole percent with DMT) CBDO and 5% (mole percent with DMT) ISB are added. The final recycled copolyester had an intrinsic viscosity of 0.690dL/g, a melting point of 212℃and a glass transition temperature of 98℃and a b value of 6.5 (results are shown in Table 1).
Comparative example 1:
as described in example 2, except that: a conventional horizontal final polycondensation reactor is used. The final regenerated copolyester had an intrinsic viscosity of 0.659dl/g, a melting point of 213.1℃and a glass transition temperature of 94℃and a b value of 9.6 (results are shown in Table 1).
Comparative example 2:
as described in example 4, except that: a conventional horizontal final polycondensation reactor is used. The final recycled copolycondensation polyester had an intrinsic viscosity of 0.652dl/g, a melting point of 208℃and a glass transition temperature of 92℃and a b value of 10.4 (results are shown in Table 1).
TABLE 1 synthetic conditions and Performance index for recycled copolyesters
Example 7:
the embodiment discloses a preparation method of regenerated DMT and copolyester thereof, which is based on the embodiment, the three-dimensional polycondensation kettle is optimally designed, the uniformity of internal materials in the reaction process can be improved, and the production of the final copolyester product is facilitated.
As shown in fig. 1, the polycondensation kettle comprises a kettle body 1, a rotating shaft 2 which is vertical in the up-down direction in the kettle body 1, a motor 3 is arranged at the upper part of the kettle body 1, the upper end of the rotating shaft 2 penetrates through the kettle body 1 and is connected with an output shaft of the motor 3, and the rotating shaft 2 can be driven to rotate through the motor 3;
two groups of stirring assemblies 4 are arranged on a rotating shaft 2 in the kettle body 1, and the two groups of stirring assemblies 4 are distributed up and down and are close to the upper end face and the lower end face of the kettle body 1; the stirring assembly 4 can be driven to rotate through the rotating shaft 2, so that materials in the kettle body 1 are stirred, and simultaneously, the stirring assembly 4 is provided with a spiral blade 43, and in the rotating process, the stirring assembly 4 can also push the materials up and down; the stirring assembly 4 on the upper side pushes down the material, the stirring assembly 4 on the lower side pushes up the material, and in the process of pushing the material by the two groups of stirring assemblies 4, the effect of circulating stirring and spiral pushing mixing is generated in the kettle body 1, so that the material in the kettle body 1 has a uniform mixing effect.
The lifting sleeve 7 is externally sleeved at the middle section of the rotating shaft 2, the supporting sleeve 5 is sleeved at the periphery of the lifting sleeve 7, the supporting sleeve 5 is fixedly arranged at the central position in the kettle body 1, the periphery of the supporting sleeve 5 is fixedly supported by the supporting rods 6, the outer ends of the supporting rods 6 are fixed on the side wall 21 of the kettle body 1, and then the supporting sleeve 5 can be fixed at the central position of the kettle body 1. The rotary support of the peripheral position of the middle section of the rotating shaft 2 is formed through the support sleeve 5, the lifting sleeve 7 between the support sleeve 5 and the rotating shaft 2 can realize up-down lifting adjustment, the rotary parameters of the stirring assembly 4 can be adjusted, and different rotary stirring effects can be realized.
As shown in fig. 1, 2 and 4, the stirring assembly 4 includes a rotating seat 41, a plurality of stirring rods 42 and paddles 43, the rotating seat 41 is fixedly mounted on the rotating shaft 2, the stirring rods 42 and paddles 43 are in one-to-one correspondence, are mounted on the periphery of the rotating seat 41, form uniform paddles 43, and the stirring rods 42 and paddles 43 can be two or more groups and are distributed in an annular circumference array. The number of stirring rods 42 and paddles 43 is illustrated as two sets.
One end of the stirring rod 42 is rotatably connected to the outer circumferential position of the rotating seat 41, and the axis of the stirring rod 42 is perpendicular to the rotating shaft 2. The paddles 43 are in one-to-one correspondence with the stirring rods 42 and are fixedly connected to one end, away from the rotating seat 41, of the stirring rods 42; by rotating the adjusting stirring rod 42, the blade 43 can also rotate relative to the rotating base 41, and the inclination angle of the blade 43 can be adjusted. In the process that the motor 3 drives the rotating shaft 2 to rotate at the same speed, the spiral pushing force of the blade 43 can be adjusted by adjusting the inclination angle of the blade 43. The stirring assembly 4 further comprises an adjusting mechanism, wherein the adjusting mechanism is arranged at the peripheral position of the rotating shaft 2 and is linked with the rotating seat 41, so that the inclination angle of the blade 43 can be adjusted.
The upper and lower two groups of stirring assemblies 4 are positioned at the positions of the kettle body 1 close to the upper and lower bottom surfaces, a certain gap position is formed at the corresponding bottom surface position, and materials in the kettle body 1 can be pushed in a spiral manner through the rotation of the stirring assemblies 4.
The blades 43 of the two sets of stirring assemblies 4 are opposite in inclination angle, and can push materials in opposite directions in the process of rotating along the rotating shaft 2. The stirring assembly 4 on the upper side can push materials downwards, and the stirring assembly 4 on the upper side can push materials upwards to form a state of pushing materials in a spiral way towards the opposite direction.
The stirring rod 42 is of a circular columnar structure, and in the rotation adjustment process, the stirring rod 42 rotates around the center, and only the material in the kettle body 1 is subjected to rotation stirring. The paddle 43 at the outer end of the stirring rod 42 is of a thin plate-shaped structure, and in the inclination adjustment process, the paddle 43 can form a spiral pushing effect on materials.
In the two sets of stirring assemblies 4, the upper side is the first stirring assembly 4, the lower side is the second stirring assembly 4, the blades 43 and the stirring rods 42 of the first stirring assembly 4 are shorter, and the blades 43 and the stirring rods 42 of the second stirring assembly 4 are longer. The length of the blade 43 of the first stirring assembly 4 is close to half of the radius of the kettle body 1, and extends to the middle position of the kettle body 1; in the first stirring assembly 4, the total length of the stirring rod 42 and the blade 43 is identical to the length of the stirring rod 42 in the second stirring assembly 4. The total length of the stirring rod 42 and the blade 43 in the first stirring assembly 4 is half of the total length of the stirring rod 42 and the blade 43 in the second stirring assembly 4. The two sets of stirring assemblies 4 form the state shown in fig. 1.
In the two groups of stirring assemblies 4, the first stirring assembly 4 mainly carries out spiral material pushing on the center position of the kettle body 1, and the second stirring assembly 4 can carry out spiral material pushing on the position, close to the side wall 21 of the kettle body 1, in the kettle body 1; the flow directions of the materials outside and the materials in the middle are opposite, a spiral circulation conveying state is formed in the reaction kettle, the mixing effect of the materials in the kettle body 1 can be greatly improved, and stable homogenization mixing treatment is formed.
As shown in fig. 2 and 4, the adjusting mechanism includes an adjusting sleeve 44 and a plurality of hinge rods 47, the adjusting sleeve 44 is sleeved outside the rotating shaft 2 and can be slidably adjusted along the axial direction of the rotating shaft 2, and in order to improve the stability of sliding adjustment, a guide groove can be arranged between the adjusting sleeve 44 and the rotating shaft 2 for adjustment so as to maintain the smoothness of adjustment of the adjusting sleeve 44.
The number of the hinge rods 47 corresponds to that of the stirring rods 42 one by one, and the position state between the adjusting sleeve 44 and the adjusting sleeve 44 can be realized through the hinge rods 47. Specifically, a first hinge seat 45 is fixedly connected to the outer peripheral position of the adjusting sleeve 44, a second hinge seat 46 is fixedly connected to the outer periphery of the stirring rod 42, and the number of the first hinge seat 45 and the number of the second hinge seat 46 are in one-to-one correspondence; two ends of the hinge rod 47 are respectively hinged between the hinge seat I45 and the hinge seat II 46, and linkage between the adjusting sleeve 44 and the stirring rod 42 is realized through the hinge rod 47.
In the up-down sliding adjustment process, the adjusting sleeve 44 can drive the stirring rod 42 to swing and adjust, and then the inclination angle of the blade 43 can be adjusted to adjust the state of pushing materials by the blade 43, and under the condition that the inclination angle of the blade 43 is large, the axial pushing action of the blade 43 can be increased during the rotating action.
An adjusting ring 410 is sleeved on the outer periphery of the adjusting sleeve 44, the adjusting ring 410 is rotationally connected with the adjusting sleeve 44 and mutually axially limited, namely, the adjusting sleeve 44 can be rotationally supported, and the adjusting sleeve 44 can be vertically adjusted through the adjusting ring 410. Specifically, two annular limiting convex rings 48 are fixedly connected to the periphery of the adjusting sleeve 44, a limiting annular groove 49 is formed between the two limiting convex rings 48, the adjusting ring 410 is rotatably sleeved in the limiting annular groove 49, and the adjusting ring is embedded into the limiting annular groove 49 to realize rotational connection and axial limiting. In order to improve the rotation smoothness between the adjusting sleeve 44 and the adjusting ring 410, a bearing may be installed between the adjusting sleeve 44 and the adjusting ring 410, so that the abrasion in the rotation process of the adjusting sleeve 44 and the adjusting ring 410 can be reduced, and the rotation smoothness between the adjusting sleeve and the adjusting ring is improved.
As shown in fig. 1 and 2, the upper and lower ends of the lifting sleeve 7 penetrate through the supporting sleeve 5 and are fixedly connected with the adjusting rings 410 of the upper and lower stirring assemblies 4 respectively. In the lifting process, the lifting sleeve 7 synchronously drives the two groups of adjusting mechanisms and drives the paddles 43 in the two groups of stirring assemblies 4 to adjust the inclination angle.
Through holes 11 for the lifting sleeve 7 to penetrate are formed in the upper end and the lower end of the supporting sleeve 5, and the through holes 11 and the lifting sleeve 7 are sealed through sliding sealing pieces. The lifting piston 8 is fixedly connected to the periphery of the lifting sleeve 7, the lifting piston 8 is positioned in the supporting sleeve 5 and is positioned in the relative middle position of the lifting sleeve 7, and a piston connecting structure is formed between the lifting piston 8 and the inner periphery of the supporting sleeve 5. The lifting piston 8 forms a sealed state, and sliding sealing members are arranged at the positions of the through holes 11 at the upper end and the lower end, so that a sealed cavity can be formed at the inner peripheral position of the supporting sleeve 5.
The lifting piston 8 is used for respectively arranging an inner cavity of the lifting sleeve 7 into an upper cavity and a lower cavity, one side of the lifting piston is provided with a pressure regulating cavity 9, the other side of the lifting piston is provided with a spring cavity 10, the regulating cavity is filled with thermal expansion liquid, the other side of the lifting piston is provided with a spring in the spring cavity 10, and the two sides of the lifting piston 8 respectively play a supporting role. The thermal expansion liquid can be kerosene or other liquid with larger thermal expansion coefficient. The thermal expansion liquid generates thermal expansion in the heating process, and then can push the lifting piston 8, thereby driving the lifting sleeve 7 and the adjusting mechanism to act. In the support cavity, the adjusting cavity and the spring cavity 10 may be both up and down, for example, the lower side may be the adjusting cavity and the upper side may be the spring cavity 10; alternatively, the upper side may be the spring chamber 10 and the lower side may be the adjustment chamber; according to the position difference of adjusting chamber and spring chamber 10, lift cover 7 also will be different in the direction that promotes in the inflation in-process, and then need also carry out suitable regulation according to direction adjustment mechanism's regulation direction to form under the normal condition, the interior thermal expansion of pressure regulating chamber 9 drives lift cover 7 and removes, and then through adjustment mechanism, increases paddle 43's inclination, and then improves paddle 43 spiral propelling movement effect.
As shown in fig. 2, the pressure regulating chamber 9 may be located at an upper side of the spring chamber 10, and the lifting piston 8 is balanced up and down by the pressure of the thermal expansion liquid and the elastic force of the spring. When the temperature of the inner cavity of the kettle body 1 is increased, the thermal expansion liquid is heated and expanded, the lifting piston 8 is pushed to overcome the spring pressure to move, the lifting sleeve 7 and the adjusting mechanism are driven to act, the inclination angle of the paddle 43 in the stirring assembly 4 is increased, and the stirring efficiency of the stirring assembly 4 is improved; when the temperature of the inner cavity of the kettle body 1 is reduced, the thermal expansion liquid contracts, the spring pushes the lifting piston 8 to move, the lifting sleeve 7 and the adjusting mechanism are driven to act, the inclination angle of the blade 43 in the stirring assembly 4 is reduced, and the stirring efficiency of the stirring assembly 4 is reduced. Under the condition of lower temperature, the circulating pushing speed is reduced, so that the thermal contact time between the material and the heating device 22 can be prolonged, and the temperature is locally increased earlier under the reasonable temperature condition, so that reaction conditions are formed; at this time, since the inclination angle of the blade 43 is small, the load applied to the entire stirring assembly 4 and the rotating shaft 2 is small, and the load of the motor 3 can be reduced.
When the temperature of the inner cavity of the kettle body 1 is lower, the up-down axial pushing effect generated by the paddle 43 is smaller, a slow and uniform circulation mixing effect can be generated, and a stable and uniform mixing effect can be formed at a low temperature; at this time, the inclination angle of the blade 43 is smaller, so that the resistance of the blade 43 is smaller in the rotation process, and the stirring assembly 4 can stably and uniformly rotate. When the temperature of the inner cavity of the kettle body 1 is increased, the blades 43 form a more deflection state due to higher temperature, so that the mixing effect of the stirring assembly 4 on materials can be improved, the efficiency of material circulating pushing in the kettle body 1 can be further improved, the circulating effect of the materials can be further accelerated, and the mixing effect of the materials can be improved.
As shown in fig. 1, 2 and 3, the support rod 6 is fixedly connected to the outer circumference of the support sleeve 5 and is positioned at a position on one side of the thermal expansion liquid. A runner 12 communicated with the inner cavity of the supporting sleeve 5 is arranged in the supporting rod 6, the runner 12 is communicated with a pressure regulating cavity 9 in the supporting sleeve 5, and a thermal expansion cavity in the supporting sleeve 5 can be communicated with an external pressure regulating device 20 through the runner 12. Through the regulating action of the pressure regulating device 20, the pressure in the pressure regulating cavity 9 can be actively regulated, so that the active regulating action is realized, and the lifting piston 8 and the lifting sleeve 7 are vertically regulated.
By adopting the pressure regulating device 20, the thermal expansion liquid in the pressure regulating cavity 9 can be directly increased or reduced so as to change the basic internal pressure in the pressure regulating cavity 9, and then the lifting sleeve 7 can be actively regulated and controlled. The pressure in the pressure regulating cavity 9 can be regulated, so that the regulating mechanism can be further regulated on the basis of thermal expansion regulation; by adjusting the pressure in the pressure adjusting chamber 9, the blade 43 can also be adjusted to the opposite inclination direction. After the adjustment, the stirring component 4 of upside can upwards spiral propelling movement material, and the stirring component 4 of downside then can downwards spiral propelling movement material, further changes the mixing promotion of stirring component 4 to the material to form more even mixed state in the middle of the internal chamber of the cauldron body 1, can promote the mixing effect and the efficiency of material through active regulatory action.
A heating device 22 is arranged in the kettle body 1, so that materials in the inner cavity of the kettle body 1 can be heated; as shown in fig. 1, the heating device 22 may be installed in the sidewall 21 of the kettle body 1 to uniformly heat the outer circumference of the kettle body 1. Since the heating is mainly performed at a position near the outer periphery of the kettle body 1, a certain temperature difference will be generated between the center of the kettle body 1 and the outer periphery.
The inner peripheral position of the side wall 21 of the kettle body 1 is fixedly provided with a liquid storage box 14, the liquid storage box 14 is of a closed cavity structure, and the inside is filled with thermal expansion liquid. The liquid storage box 14 is fixedly connected with the support rod 6, the support rod 6 is internally provided with a flow channel 12, and the pressure regulating cavity 9 is communicated with the liquid storage box 14 through the flow channel 12, so that the thermal expansion liquid in the two chambers can generate mutual pressure regulating effect.
The peripheral liquid storage box 14 is closer to the heating device 22, a certain temperature difference exists between the liquid storage box 14 and the pressure regulating cavity 9, and in the heating process, after the liquid storage box 14 detects the heating condition, thermal expansion is generated earlier, and the pressure in the pressure regulating cavity 9 is directly transmitted to the pressure regulating cavity 9. Under the hydraulic action in the pressure regulating cavity 9, the lifting sleeve 7 is driven to move and regulate, and the blade 43 is driven to deflect by the regulating mechanism, so that the spiral pushing effect of the blade 43 is improved. The liquid source in the middle of the pressure regulating cavity 9 can be connected to the position nearby the periphery of the kettle body 1 through the liquid storage box 14 and the flow channel 12, so that the pressure regulating cavity 9 in the center of the kettle body 1 can be more easily affected by pressure, and the thermal inductance regulating efficiency of the thermal expansion liquid is improved.
The outside position of the liquid storage box 14 is connected with a conduit 18, the conduit 18 penetrates through the side wall 21 of the kettle body 1 and extends out of the kettle body 1, a solenoid valve II 19 is arranged on the conduit 18, and the conduit 18 is connected to an external pressure regulating device 20. The pressure in the liquid storage box 14 and the pressure regulating cavity 9 can be regulated through the pressure regulating device 20 so as to regulate the total amount of the thermal expansion liquid in the pressure regulating cavity 9 and the liquid storage box 14, and then the lifting piston 8 and the lifting piston can be regulated in a lifting way. In addition to thermal expansion and contraction, the inclination angle of the blade 43 can be further adjusted by actively performing an adjustment operation by the pressure adjusting device 20.
Further, a balance cavity 16 is formed by expanding the middle section of the flow channel 12 in the support rod 6, the balance cavity 16 is in a cylindrical structure, two ends of the balance cavity 16 are connected into the flow channel 12, and a balance piston 17 is connected with a piston in the balance cavity 16; the balance piston 17 can balance the pressure in the flow channel 12, and the balance piston 17 has a sliding forming range in the balance cavity 16, so that the pressure in the access pressure storage cavity can be regulated and limited, and excessive regulation of the pressure in the pressure regulating cavity 9 is avoided, and excessive regulation of the stirring assembly 4 is avoided, so that the regulation stable state of the stirring assembly 4 is maintained.
The first electromagnetic valve 13 is arranged on the runner 12 of the supporting rod 6, the first electromagnetic valve 13 is positioned at the runner 12 between the balance cavity 16 and the pressure regulating cavity 9, and the on-off of the runner 12 in the supporting rod 6 can be regulated and controlled through the first electromagnetic valve 13. The first electromagnetic valve 13 is closed, the flow channel 12 can be closed, the pressure regulating cavity 9 is connected into the balance cavity 16 and the liquid storage box 14, and the temperature of the center of the kettle body 1 is only adjusted at the moment; the first electromagnetic valve 13 is opened, the flow channel 12 can be opened, the pressure regulating cavity 9 and the flow channel 12 can be closed, and the heat conduction balance effect can be achieved at the inner and outer positions of the drawing. The expansion condition of the pressure in the pressure regulating cavity 9 can be adjusted by switching the on-off of the first electromagnetic valve 13, and the pressure regulating cavity 9 is independently expanded and adjusted, and the pressure regulating cavity 9 and the liquid storage box 14 are in linkage adjustment to switch, so that the uniform action of the stirring assembly 4 is controlled.
By adopting the reaction kettle device, the raw materials in the copolyester production process can be subjected to homogenization mixing treatment, the mixing rate of each material is regulated according to the temperature change condition in the mixing reaction process, the material heating and mixing homogenization degree in the mixing reaction process is kept, and the efficient and stable mixing effect is achieved.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (9)
1. The polycondensation kettle device for regenerating DMT and copolyester thereof is characterized by comprising a kettle body (1), wherein a rotating shaft (2) is vertical in the up-down direction in the kettle body (1), and the rotating shaft (2) is driven to rotate by a motor (3); two groups of stirring assemblies (4) are arranged on a rotating shaft (2) in the kettle body (1), each stirring assembly (4) comprises a rotating seat (41), a plurality of stirring rods (42) and paddles (43), the rotating seats (41) are fixedly arranged on the rotating shaft (2), the stirring rods (42) and the paddles (43) are in one-to-one correspondence, the stirring rods (42) and the paddles (43) are two groups, and the stirring assemblies are arranged on the periphery of the rotating seat (41) and are in a state of annular circumference whole row distribution;
the inclination angles of the paddles (43) of the two groups of stirring assemblies (4) are opposite, the stirring assembly (4) on the upper side can push materials downwards, and the stirring assembly (4) on the upper side can push materials upwards;
the stirring assembly (4) further comprises an adjusting mechanism, wherein the adjusting mechanism is arranged at the peripheral position of the rotating shaft (2) and is linked with the rotating seat (41), so that the inclination angle of the blade (43) can be adjusted; the adjusting mechanism comprises an adjusting sleeve (44) and a plurality of hinging rods (47), wherein the adjusting sleeve (44) is sleeved outside the rotating shaft (2) and can axially slide and adjust along the rotating shaft (2); the number of the hinging rods (47) corresponds to that of the stirring rods (42) one by one, and the positions between the adjusting sleeves (44) and the adjusting sleeves (44) can be realized through the hinging rods (47); the outer circumference of the adjusting sleeve (44) is fixedly connected with a first hinging seat (45), the outer circumference of the stirring rod (42) is fixedly connected with a second hinging seat (46), two ends of the hinging rod (47) are respectively hinged between the first hinging seat (45) and the second hinging seat (46), and linkage between the adjusting sleeve (44) and the stirring rod (42) is realized through the hinging rod (47); in the up-down sliding adjustment process, the adjusting sleeve (44) can drive the stirring rod (42) to swing and adjust, so that the inclination angle of the blade (43) can be adjusted.
2. The polycondensation reactor apparatus for regenerating DMT and its copolyester according to claim 1, wherein the outer circumference of the adjusting sleeve (44) is sleeved with an adjusting ring (410), the adjusting ring (410) is rotatably connected with the adjusting sleeve (44), and is axially limited with each other, and the adjusting sleeve (44) is adjusted up and down by the adjusting ring (410).
3. The polycondensation kettle device for regenerating DMT and copolyester thereof according to claim 2, wherein a lifting sleeve (7) is externally sleeved at the middle section of the rotating shaft (2), a supporting sleeve (5) is sleeved at the periphery of the lifting sleeve (7), the supporting sleeve (5) is fixedly arranged at the central position in the kettle body (1), and the periphery of the supporting sleeve (5) is supported and fixed through a supporting rod (6); the upper end and the lower end of the lifting sleeve (7) penetrate through the supporting sleeve (5) and are fixedly connected with the adjusting rings (410) of the upper stirring assembly and the lower stirring assembly (4) respectively; in the lifting process, the lifting sleeve (7) drives the blades (43) in the two groups of adjusting mechanisms (4) to adjust the dip angle.
4. A polycondensation kettle device for regenerating DMT and copolyester thereof according to claim 3, wherein the upper end and the lower end of the supporting sleeve (5) are respectively provided with a through hole (11) for the lifting sleeve (7) to penetrate, and the through holes (11) and the lifting sleeve (7) are sealed by a sliding sealing piece; the periphery of the lifting sleeve (7) is fixedly connected with a lifting piston (8), the lifting piston (8) is positioned in the supporting sleeve (5) and is positioned in the relative middle position of the lifting sleeve (7), and a piston connecting structure is formed between the lifting piston (8) and the inner periphery of the supporting sleeve (5); the lifting piston (8) forms a sealed state, sliding sealing pieces are arranged at the positions of through holes (11) at the upper end and the lower end, and a sealed cavity is formed at the inner peripheral position of the supporting sleeve (5).
5. The polycondensation kettle device for regenerating DMT and copolyester thereof according to claim 3, wherein the lifting piston (8) is characterized in that the inner cavity of the lifting sleeve (7) is respectively provided with an upper cavity and a lower cavity, one side is provided with a pressure regulating cavity (9), the other side is provided with a spring cavity (10), the regulating cavity is filled with thermal expansion liquid, the spring cavity (10) at the other side is internally provided with springs, and the two sides of the lifting piston (8) are respectively provided with a supporting function; in the heating process of the thermal expansion liquid, thermal expansion is generated, the lifting piston (8) is pushed, and the lifting sleeve (7) and the regulating mechanism are driven to act.
6. The polycondensation reactor apparatus for regenerating DMT and its copolyester according to claim 5, wherein the pressure regulating chamber (9) is located at the upper side of the spring chamber (10), and the lifting piston (8) is balanced up and down by the pressure of the thermal expansion liquid and the elasticity of the spring; when the temperature of the inner cavity of the kettle body (1) is increased, the thermal expansion liquid is heated and expanded, the lifting piston (8) is pushed to overcome the spring pressure to move, the lifting sleeve (7) and the regulating mechanism are driven to act, the inclination angle of the blade (43) in the stirring assembly (4) is increased, and the stirring efficiency of the stirring assembly (4) is improved; when the temperature of the inner cavity of the kettle body (1) is reduced, the thermal expansion liquid contracts, the spring pushes the lifting piston (8) to move, the lifting sleeve (7) and the adjusting mechanism are driven to act, the inclination angle of the blade (43) in the stirring assembly (4) is reduced, and the stirring efficiency of the stirring assembly (4) is reduced.
7. The polycondensation kettle device for regenerating DMT and copolyester thereof according to claim 6, wherein the supporting rod (6) is fixedly connected to the periphery of the supporting sleeve (5) and is positioned at one side of the thermal expansion liquid, a runner (12) communicated with the inner cavity of the supporting sleeve (5) is arranged in the supporting rod (6), the runner (12) is communicated with a pressure regulating cavity (9) in the supporting sleeve (5), and the thermal expansion cavity in the supporting sleeve (5) can be communicated with an external pressure regulating device (20) through the runner (12).
8. The polycondensation reactor apparatus for regenerating DMT and its copolyesters according to claim 6, wherein a heating device (22) is installed in the reactor body (1), and the heating device (22) is installed in the side wall (21) of the reactor body (1); a liquid storage box (14) is fixedly arranged at the inner peripheral position of the side wall (21) of the kettle body (1), the liquid storage box (14) is of a closed cavity structure, and the inside is filled with thermal expansion liquid; the liquid storage box (14) is fixedly connected with the support rod (6), a flow channel (12) is arranged in the support rod (6), and the pressure regulating cavity (9) is communicated with the liquid storage box (14) through the flow channel (12).
9. The polycondensation reactor apparatus for regenerating DMT and its copolyesters according to claim 8, wherein the outer side of the liquid storage box (14) is connected with a conduit (18), the conduit (18) penetrates through the side wall (21) of the reactor body (1) and extends to the outer side of the reactor body (1), a solenoid valve two (19) is installed on the conduit (18), and the conduit (18) is connected to an external pressure regulating device (20).
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