CN103146151B - Recycling method of waste polyester bottle - Google Patents
Recycling method of waste polyester bottle Download PDFInfo
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- CN103146151B CN103146151B CN201110401312.XA CN201110401312A CN103146151B CN 103146151 B CN103146151 B CN 103146151B CN 201110401312 A CN201110401312 A CN 201110401312A CN 103146151 B CN103146151 B CN 103146151B
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- 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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Abstract
The invention discloses recycling method of a waste polyester bottle. The method comprises: (1) a polymerization system of recycling; and (2) a purifying system of by-product collection and solvent recycling. The method continuously treats the waste polyester bottle sheets, so that produced POY filament recycled from the waste polyester bottle can be used in a field of high-strength industrial yarn, produced short fibers can be used in a field of nonwovens, and produced slices can be used in a filed of polyester bottles, thereby realizing a large-scale high-value-added recycling of the waste polyester bottles, satisfying market requirements, reducing industry's dependence on oil. The method can save energy, protect environment, promote a continuous development of polyester industry, and develop a circular economy.
Description
Technical field
The invention belongs to resource recovery field, more specifically, the present invention relates to a kind of method of waste polyester bottle recycling, the method is for continuous treatment waste polyester bottle and makes it be recycled the industrial recovery method of recycling.
Background technology
Polyester (PET), chemistry polyethylene terephthalate by name, being commonly called as terylene, is one of several plastics be most widely used at present.As thermoplastic film field, it is one of best several prods of physical strength and toughness.Excellent in cushion effect, wear resisting property is good, has good creep resistant, and rigidity is strong, hardness is large, product surface good luster, transparency is high, and water-absorbent is lower, and chemical-resistant reagent box oil-proofness is good, physical and mechanical properties can not lost in wide temperature range, can for a long time 120 DEG C of uses, these excellent over-all propertieies make it be widely used at packaging industry, are used in particular for producing drink bottle, oil can etc.And these products disposable field consumption is in the majority, but cause it can not be degraded by external microbe within considerable time due to these excellent performances of polyester.Cause a new round " white pollution " and " space-pollution ", the especially anxiety of oil, had a strong impact on again the production of polyester bottles.Therefore, large-scale Pillar recovery bottle recycling has very urgent.
The recycling of polyester bottles is field very important during polymer is recycled.Waste polyester bottle recovery technology is divided into physiochemical mutagens technology and the large class of chemical recovery techniques two.Physiochemical mutagens is by waste polyester heating and melting, and by screw extruder extrusion moulding after purifying, general process is: classification-fragmentation-cleaning-dehydration-drying-granulation (spinning).Chemical recovery method is, by chemical reaction, waste polyester is depolymerized to low molecular compound as terephthalic acid (TPA), dimethyl terephthalate (DMT) (DMT), ethylene glycol terephthalate (BHET), the different new ester (DOTP) of terephthalic acid two, L--alcohol (EG) etc., again as polyester raw material, or other products can be made after alcoholysis product is purified.Chemical recovery method also comprises chemistry to be improved, and employing chain modification usually, cross-linking modified, chlorination modified etc. changes chain length, the structure of polyester, thus improves its some characteristic.
At present, reclaim field development rapidly both at home and abroad at waste polyester bottle, the such as U.S. utilizes useless PET bottle through Methanolysis, production dimethyl terephthalate (DMT) and hexylene glycol, more directly carries out polycondensation and prepare new polyester.These major parts are all carry out recovery degradation according to the Application Areas originally of raw material to use.Recently the technology that " bottle " arrives " bottle " is also developed, " bottle " arrives the technology of " fiber ", but the section of regeneration is still mixed in primary section by the technology of these " bottles " to " bottle ", " bottle " to " fiber " is also that degradation uses mostly, and the uniformity requirements of technique to the water ratio of returnable bottle, viscosity is too high, single complete equipment capacity does not have room for promotion, and the solvent toxicity adopted in addition is strong, does not provide the cleaning manufacturing technique method that solvent cycle utilizes.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of waste polyester bottle recycling method, the method can reclaim obtain high viscosity, high added value the polyester POY long filament that can be used for industrial yarn, for Nonwovens Field staple fibre and be back to PET bottle grade chip again, realize the recycle of recycling design simultaneously, ensure that the cleaner production of this industrialization technology.
The present invention is realized by following technical scheme:
A method for waste polyester bottle recycling, it comprises the following steps:
(1) paradigmatic system of recycling;
(2) purification system that by product is collected and solvent cycle utilizes.
The paradigmatic system of the recycling in described step (1) comprises the following steps:
(1) waste polyester bottle melting alcoholysis system;
(2) polycondensation system;
(3) Masterbatch injected system;
The purification systems that by product in described step (2) is collected and solvent cycle utilizes comprises the following steps:
(1) ethylene glycol extracted out from the alcoholysis still of the paradigmatic system of recycling enters an ethylene glycol lightness-removing column, removes the light constituent in alcoholysis ethylene glycol, in overhead collection to light constituent, obtains not containing the ethylene glycol of light constituent at the bottom of tower;
(2) ethylene glycol after the process of ethylene glycol lightness-removing column enters an ethylene glycol weight-removing column and processes, and the heavy constituent at the bottom of tower is carried out collection and treatment, obtains at tower top the ethylene glycol that purity is greater than 85%;
(3) four parts are divided into from ethylene glycol weight-removing column high purity ethylene glycol out: first part removes alcoholysis still, for alcoholysis melting operation provides alcoholysis ethylene glycol, second section removes the squirt pump of vacuum system through the ethylene glycol vaporizer of vacuum system, Part III enters ethylene glycol squirt pump hot well, and last part gets back to fresh ethylene glycol storage tank;
(4) ethylene glycol of ethylene glycol squirt pump hot well inputs the ethylene glycol hot well of whole polycondensation vessel through pump, and the ethylene glycol for whole polycondensation vessel sprays;
(5) the ethylene glycol hot well overflow of whole polycondensation vessel enters precondensation moral ethylene glycol hot well, and the ethylene glycol for precondensation still sprays, and in the ethylene glycol that this part produces, other component concentration is higher, returns ethylene glycol lightness-removing column and carries out circular treatment;
(6) spent glycol storage tank constantly supplements the amount of the ethylene glycol that whole device consumes, and part is delivered to retrieving arrangement use simultaneously, forms the system of a circulation closed.
Another aspect of the present invention, described step waste polyester bottle melting alcoholysis system comprises the steps:
(1) enter screw rod melting through feed bin after waste polyester bottle fragmentation, add alcoholysis ethylene glycol toward screw rod simultaneously and carry out partial alcoholysis to it, the amount of heated glycol is the 5%-1000% of waste polyester bottle quality, and the temperature of screw rod melting alcoholysis is 150-260 DEG C;
(2) material be melting out through screw rod enters alcoholysis still, carry out further alcoholysis, ensure that the abundant alcoholysis of waste polyester bottle raw material, this stage alcoholysis is carried out under certain vacuum tightness, the vacuum tightness of this alcoholysis process is absolute pressure 1000Pa-10000Pa, and the ethylene glycol of extraction enters the process of ethylene glycol lightness-removing column.
Another aspect of the present invention, described step polycondensation system comprises the steps:
(1) material after the further alcoholysis of alcoholysis still enters three phases and precondensation stage, or/and add catalyzer to deviate from the small molecules in alcoholysate before entering precondensation stage, carry out partially polymerized to reduce the pressure that whole polycondensation vessel needs to increase substantially material viscosity simultaneously, this stage needs carry out under certain negative pressure, the temperature of this process controls at 250-280 DEG C, and vacuum tightness is absolute pressure 1000Pa-5000Pa;
(2) material after precondensation stage process enters whole polycondensation phase, and final minification is poly-adopts thickening still, and deviate from ethylene glycol and other small molecules, the temperature of this process controls at 250-295 DEG C, and its vacuum degree control is absolute pressure 50Pa-500Pa.
Another aspect of the present invention, described Masterbatch injected system is by described Masterbatch and polycondensation melt-mixing out.
Beneficial effect of the present invention is:
The method of waste polyester bottle recycling disclosed by the invention, the serialization recycling of extensive waste polyester bottle will be realized, through engineering approaches is strong, can produce high viscosity, high added value the polyester POY long filament that can be used for industrial yarn, for the staple fibre of non-woven and the bottle grade pet chip of reuse again.The uniformity requirements of this technique to the water ratio of returnable bottle, viscosity is not high, single complete equipment capacity boost space is large, and the solvent adopted in removal process can recycle, method of the present invention can reduce the degree of dependence of PET industry to oil, reduces industrial goods production discharge capacity.Decrease pollution, enabling environment is protected simultaneously, promotes the Sustainable development of PET industry.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of waste polyester bottle recycling;
Fig. 2 is the recycle process for cleanly preparing schema of solvent for use.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
As shown in Figure 1, take waste polyester bottle 1000kg/h, enter screw rod melting, add ethylene glycol 100kg/h, alcoholysis 30min at normal pressure, temperature are 190 DEG C toward screw rod, the material be melting out through screw rod enters alcoholysis still simultaneously, further alcoholysis is carried out under tiny structure, temperature is alcoholysis 10min at 200 DEG C, ensure that the abundant alcoholysis of Waste Polyester raw material, and the ethylene glycol that this stage extracts out enters ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, catalyzer 1g is added before entering precondensation stage, the catalyst glycol concentration be made into is 20%, be 2000Pa in vacuum tightness, temperature of reaction is 275 DEG C, be 60min between reaction is seasonable, deviate from the small molecules in alcoholysate, simultaneously partially polymerized, material after precondensation process enters final minification and gathers, at vacuum tightness < 300Pa, temperature of reaction is 285 DEG C, be 90min between reaction is seasonable, deviate from the small molecules such as ethylene glycol, obtain the limiting viscosity > 0.67dl/g of the polyester regenerated.
Embodiment 2
As shown in Figure 1, take waste polyester bottle 1000kg/h, enter screw rod melting, add ethylene glycol 100kg/h, alcoholysis 30min at normal pressure, temperature are 190 DEG C toward screw rod, the material be melting out through screw rod enters alcoholysis still simultaneously, further alcoholysis is carried out under tiny structure, temperature is alcoholysis 20min at 200 DEG C, ensure that the abundant alcoholysis of Waste Polyester raw material, and the ethylene glycol that this stage extracts out enters ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, catalyzer 1g is added before entering precondensation stage, the catalyst glycol concentration be made into is 20%, be 1000Pa in vacuum tightness, temperature of reaction is 275 DEG C, be 60min between reaction is seasonable, deviate from the small molecules in alcoholysate, simultaneously partially polymerized, material after precondensation process enters final minification and gathers, at vacuum tightness < 50Pa, temperature of reaction is 285 DEG C, be 100min between reaction is seasonable, deviate from the small molecules such as ethylene glycol, obtain the limiting viscosity > 0.85dl/g of the polyester regenerated.
Embodiment 3
As shown in Figure 1, take waste polyester bottle 1200kg/h, enter screw rod melting, add ethylene glycol 150kg/h, alcoholysis 30min at normal pressure, temperature are 190 DEG C toward screw rod, the material be melting out through screw rod enters alcoholysis still simultaneously, further alcoholysis is carried out under tiny structure, temperature is alcoholysis 20min at 200 DEG C, ensure that the abundant alcoholysis of Waste Polyester raw material, and the ethylene glycol that this stage extracts out enters ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, catalyzer 1g is added before entering precondensation stage, the catalyst glycol concentration be made into is 20%, be 1000Pa in vacuum tightness, temperature of reaction is 275 DEG C, be 60min between reaction is seasonable, deviate from the small molecules in alcoholysate, simultaneously partially polymerized, material after precondensation process enters final minification and gathers, at vacuum tightness < 50Pa, temperature of reaction is 285 DEG C, be 100min between reaction is seasonable, deviate from the small molecules such as ethylene glycol, obtain the limiting viscosity > 0.85dl/g of the polyester regenerated.
Embodiment 4
As shown in Figure 1, take waste polyester bottle 1000kg/h, enter screw rod melting, add ethylene glycol 100kg/h, alcoholysis 30min at normal pressure, temperature are 190 DEG C toward screw rod, the material be melting out through screw rod enters alcoholysis still simultaneously, further alcoholysis is carried out under tiny structure, temperature is alcoholysis 20min at 200 DEG C, ensure that the abundant alcoholysis of Waste Polyester raw material, and the ethylene glycol that this stage extracts out enters ethylene glycol treatment system.Material after the further alcoholysis of alcoholysis still enters precondensation stage, catalyzer 1g is added before entering precondensation stage, the catalyst glycol concentration be made into is 20%, be 1500Pa in vacuum tightness, temperature of reaction is 275 DEG C, be 60min between reaction is seasonable, deviate from the small molecules in alcoholysate, simultaneously partially polymerized, material after precondensation process enters final minification and gathers, at vacuum tightness < 50Pa, temperature of reaction is 285 DEG C, be 100min between reaction is seasonable, deviate from the small molecules such as ethylene glycol, obtain the limiting viscosity > 0.80dl/g of the polyester regenerated.
Embodiment 5
The ethylene glycol 120kg/h that the alcoholysis still carrying out autonomous technique retrieving arrangement is extracted out, enter the process of an ethylene glycol lightness-removing column, remove the light constituent in alcoholysis ethylene glycol, overhead collection to light constituent and by this part light constituent collect carry out export trade process, at the bottom of tower, obtained the ethylene glycol 118kg/h of light constituent, enter an ethylene glycol weight-removing column to process, heavy constituent at the bottom of tower is carried out collection export trade process, obtain highly purified ethylene glycol 114kg/h at tower top, purity is > 85%.
Should be appreciated that and above describe for the present invention to be as set forth in the claims only example and illustrative, not to be limited it.Content of the present invention disclosed by this paper, other embodiment of the present invention is apparent for a person skilled in the art.It should be noted that this specification sheets and embodiment only should be seen as example, actual range of the present invention should be determined by claim.
Claims (1)
1. a method for waste polyester bottle recycling, is characterized in that: it comprises following two large treatment systems:
(A) paradigmatic system of recycling;
(B) purification system that by product is collected and solvent cycle utilizes;
The paradigmatic system of described (A) recycling comprises following three treatment systems:
(1) waste polyester bottle melting alcoholysis system;
(2) polycondensation system;
(3) Masterbatch injected system;
The purification system that described (B) by product is collected and solvent cycle utilizes comprises the following steps:
(1) ethylene glycol extracted out from the alcoholysis still of the paradigmatic system of recycling enters an ethylene glycol lightness-removing column, removes the light constituent in alcoholysis ethylene glycol, in overhead collection to light constituent, obtains not containing the ethylene glycol of light constituent at the bottom of tower;
(2) ethylene glycol after the process of ethylene glycol lightness-removing column enters an ethylene glycol weight-removing column and processes, and the heavy constituent at the bottom of tower is carried out collection and treatment, obtains at tower top the ethylene glycol that purity is greater than 85%;
(3) four parts are divided into from ethylene glycol weight-removing column high purity ethylene glycol out: first part removes alcoholysis still, for alcoholysis melting operation provides alcoholysis ethylene glycol, second section removes the squirt pump of vacuum system through the ethylene glycol vaporizer of vacuum system, Part III enters ethylene glycol squirt pump hot well, and last part gets back to fresh ethylene glycol storage tank;
(4) ethylene glycol of ethylene glycol squirt pump hot well inputs the ethylene glycol hot well of whole polycondensation vessel through pump, and the ethylene glycol for whole polycondensation vessel sprays;
(5) the ethylene glycol hot well overflow of whole polycondensation vessel enters the ethylene glycol hot well of precondensation still, and the ethylene glycol for precondensation still sprays, and in the ethylene glycol that this part produces, other component concentration is higher, returns ethylene glycol lightness-removing column and carries out circular treatment;
(6) spent glycol storage tank constantly supplements the amount of the ethylene glycol that whole device consumes, and part is delivered to retrieving arrangement use simultaneously, forms the system of a circulation closed;
Described (one) waste polyester bottle melting alcoholysis system comprises the steps:
(1) enter screw rod melting through feed bin after waste polyester bottle fragmentation, add alcoholysis ethylene glycol toward screw rod simultaneously and carry out partial alcoholysis to it, the amount of heated glycol is the 5%-1000% of waste polyester bottle quality, and the temperature of screw rod melting alcoholysis is 150-260 DEG C;
(2) material be melting out through screw rod enters alcoholysis still, carry out further alcoholysis, ensure that the abundant alcoholysis of waste polyester bottle raw material, this stage alcoholysis is carried out under certain vacuum tightness, the vacuum tightness of this alcoholysis process is absolute pressure 1000Pa-10000Pa, and the ethylene glycol of extraction enters the process of ethylene glycol lightness-removing column;
Described (two) polycondensation system comprises the steps:
(1) material after the further alcoholysis of alcoholysis still enters three phases and precondensation stage, or/and add catalyzer to deviate from the small molecules in alcoholysate before entering precondensation stage, carry out partially polymerized to reduce the pressure that whole polycondensation vessel needs to increase substantially material viscosity simultaneously, this stage needs carry out under certain negative pressure, the temperature of this process controls at 250-280 DEG C, and vacuum tightness is absolute pressure 1000Pa-5000Pa;
(2) material after precondensation stage process enters whole polycondensation phase, and final minification is poly-adopts thickening still, and deviate from ethylene glycol and other small molecules, the temperature of this process controls at 250-295 DEG C, and its vacuum degree control is absolute pressure 50Pa-500Pa;
Described (three) Masterbatch injected system be by described Masterbatch and polycondensation after melt-mixing.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110401312.XA CN103146151B (en) | 2011-12-06 | 2011-12-06 | Recycling method of waste polyester bottle |
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| CN201110401312.XA CN103146151B (en) | 2011-12-06 | 2011-12-06 | Recycling method of waste polyester bottle |
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| CN103146151B true CN103146151B (en) | 2015-04-08 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103342832B (en) * | 2013-07-13 | 2015-01-28 | 福建锦兴环保科技有限公司 | Recovery device and recovery process of waste polyester bottle flakes |
| CN103357605B (en) * | 2013-07-13 | 2015-04-15 | 福建锦兴环保科技有限公司 | Cleaning device and process for waste polyester bottle chip |
| CN106609405A (en) * | 2015-10-23 | 2017-05-03 | 南通金康弘纺织品有限公司 | Method for recovery and reutilization of waste cotton textile |
| CN107459788B (en) * | 2017-07-20 | 2019-05-24 | 东华大学 | A kind of regeneration method of polyester reclaiming material |
| CN107523895B (en) * | 2017-07-20 | 2019-01-11 | 东华大学 | A kind of coloured regenerative polyester staple fiber and preparation method thereof |
| CN107523892B (en) * | 2017-07-20 | 2019-01-15 | 东华大学 | A kind of Regenerated Polyester Fibres and preparation method thereof |
| CN111472059B (en) * | 2020-04-16 | 2021-10-08 | 莱芜富新纤维制品有限公司 | Production line of polyester staple fibers |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805445A (en) * | 2010-01-29 | 2010-08-18 | 成强 | Chemical treating method for melt polycondensation high polymer old material regeneration |
| CN102153734A (en) * | 2010-12-30 | 2011-08-17 | 金发科技股份有限公司 | Method for preparing biodegradable polyester from consumed polyester |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805445A (en) * | 2010-01-29 | 2010-08-18 | 成强 | Chemical treating method for melt polycondensation high polymer old material regeneration |
| CN102153734A (en) * | 2010-12-30 | 2011-08-17 | 金发科技股份有限公司 | Method for preparing biodegradable polyester from consumed polyester |
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