CN1239461C - Microwave depolymerization method for PET - Google Patents
Microwave depolymerization method for PET Download PDFInfo
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- CN1239461C CN1239461C CNB2004100254964A CN200410025496A CN1239461C CN 1239461 C CN1239461 C CN 1239461C CN B2004100254964 A CNB2004100254964 A CN B2004100254964A CN 200410025496 A CN200410025496 A CN 200410025496A CN 1239461 C CN1239461 C CN 1239461C
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- pet
- microwave
- reaction
- polyethylene terephthalate
- pure water
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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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- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The present invention discloses a microwave depolymerization method for PET, which has mild reaction condition and simple after-treatment process. Pure water is used as a depolymerizing agent, a certain amount of PET and the pure water are put in a reactor by the weight ratio of 10:1 and generate reaction by microwave radiation at the temperature of 220 to 230 DEGC and the pressure of 2.0 to 2.5MPa, the time of microwave radiation is 120 to 60 min so that the PET can be completely depolymerized. The microwave depolymerization method can realize the cyclic utilization of PET polyester.
Description
Technical field
The present invention relates to the depolymerization method of a kind of PET, particularly the microwave depolymerization method of PET.
Background technology
PET (polyethylene terephthalate) is widely used in fields such as beverage bottle, fiber, film, sheet base and electrical apparatus insulation material with its excellent performance.The fast development of polyester industrial, incident is the sharp increase of polyester waste material, for example China has formed huge beverage market in recent years, nearly approximately 10,000,000,000 of year consumption PET bottle, as not in addition reasonably recycle, not only cause the huge wasting of resources, and produce the serious environmental pollution.Chemical depolymerization is to be monomer (as terephthalic acid TPA, dimethyl terephthalate (DMT) DMT, diglycol terephthalate BHET, ethylene glycol EG) or other chemical with the depolymerization of PET polyester waste material, behind separation, purifying, can be again as raw material or other industrial chemicals of polyester, thereby realizing the utilization of PET resource circulation, also is uniquely can realize the recycle of PET polyester, the method for producing again.At present the chemical depolymerization method of PET mainly contains hydrolysis method, alcoholysis method etc., and hydrolysis method need add acid or alkali as catalyzer, has spent acid solution, waste lye to discharge in the reaction process, contaminate environment, and to carry out product and catalyzer separate complex process; Alcoholysis method needs high temperature, high pressure, realizes difficulty on the technology, and needs catalyzer, brings certain difficulty to separation.
The A.Krzan of Yugoslav has studied the alcoholysis reaction of PET under the microwave action, and under catalyst action, PET is depolymerization fully in 10min.But this method has only solved the problem of severe reaction conditions in the alcoholysis method, because the existence of catalyzer is arranged, has the problem of aftertreatment difficulty equally.
Summary of the invention
The purpose of this invention is to provide a kind of reaction conditions gentleness, the simple PET microwave of last handling process depolymerization method.
For achieving the above object, the present invention is by the following technical solutions: the microwave depolymerization method of a kind of PET, make depolymerizing agent with pure water, with a certain amount of PET and pure water with pure water: PET=10: 1 weight ratio is put into reactor, under 220～230 ℃ of temperature, pressure 2.0～2.5MPa condition, react microwave irradiation time 120～60min, PET depolymerization fully with microwave radiation.
In the above technical scheme, the depolymerization reaction of PET in pure water comes down to the inverse process that polycondensation prepares PET (small molecule by-product is a water), depolymerization reaction generates solid-state terephthalic acid (TPA) and liquid ethylene glycol (EG), owing to do not introduce other material in the reaction process, product is filtered, solid-state terephthalic acid (TPA) can be separated with liquid ethylene glycol (EG),, thereby realize the utilization of PET resource circulation again as raw material or other industrial chemicals of polyester.Therefore the depolymerization method of PET of the present invention will be eliminated the numerous unfavorable factors that exist in the present PET depolymerization method: severe reaction conditions (high temperature, high pressure), sepn process complexity (acid, alkali, catalyzer etc.), last handling process are to the pollution of environment etc.
Further specify the present invention below by embodiment.
Embodiment
Embodiment 1
Laboratory apparatus: reactor is ETHOS 900 microwave devices (Italy); EQUINOX55 infrared spectrometer (Germany); PERKIN ELMER gas-chromatography (U.S.).
Experiment reagent: PET is the waste polyester beverage bottle; Pure water is a redistilled water; Other is analytical reagent.
Experimental technique:
The PET polyester chips is cut into lamellar body of uniform size, and (5mm * 5mm), washing is also dry, with a certain amount of PET (m
1) and pure water put into reactor, setting reaction conditions (220 ℃ of temperature, pressure 2.0MPa, microwave power 600Watt) begins to react, after the microwave radiation reaction 120min, with reactor cooling, then product is filtered, wash solid with less water simultaneously, solid 40 ℃ of following vacuum-dryings to constant weight, with 10%NaOH solution dissolving after-filtration, insolubles to constant weight, is designated as m through washing, drying under reduced pressure
2, the method for calculation of PET depolymerization rate are (m
1-m
2)/m
1* 100%.The liquid gas chromatographic analysis, gas-chromatography adopts marker method and external standard method, and analytical results shows the glycol ether that contains ethylene glycol and trace in the liquid.Solid at first with the dissolving of NaOH solution, filtration, refilters behind the adding sulfuric acid acidation (TPA is separated out), vacuum-drying, and solid IR spectrogram is consistent with the standard spectrogram of TPA behind the purifying, proves that solid is TPA.Occurring a spot of glycol ether in the depolymerization product is because have in the polyester molecule chain due to a spot of glycol ether unit.Experimental result is as shown in table 1.
Table 1
| The embodiment sequence number | Temperature of reaction (℃) | Microwave power (Watt) | Reaction pressure (MPa) | Reaction times (minute) | Depolymerization rate (%) |
| 1 2 3 | 220 225 230 | 600 600 600 | 2.0 2.5 2.3 | 120 90 60 | 100.0 100.0 100.0 |
Annotate: PET: pure water=1: 10 (wt%)
Embodiment 2
Reaction conditions is set at 225 ℃ of temperature, pressure 2.5MPa, microwave power 600Watt, and the reaction times is 90min, and experimental technique is with embodiment 1, and experimental result is as shown in table 1.
Embodiment 3
Reaction conditions is set at 230 ℃ of temperature, pressure 2.3MPa, microwave power 600Watt, and the reaction times is 60min, and experimental technique is with embodiment 1, and experimental result is as shown in table 1.
Claims (4)
1, a kind of microwave depolymerization method of polyethylene terephthalate, it is characterized in that: make depolymerizing agent with pure water, with a certain amount of polyethylene terephthalate and pure water with pure water: the weight ratio of polyethylene terephthalate=10: 1 is put into reactor, under 220～230 ℃ of temperature, pressure 2.0～2.5MPa condition, react with microwave radiation, microwave irradiation time 120～60min, the polyethylene terephthalate depolymerization forms terephthalic acid and ethylene glycol.
2, the microwave depolymerization method of polyethylene terephthalate according to claim 1 is characterized in that: 220 ℃ of temperature of reaction, reaction pressure 2.0MPa, microwave irradiation time 120min.
3, the microwave depolymerization method of polyethylene terephthalate according to claim 1 is characterized in that: 225 ℃ of temperature of reaction, reaction pressure 2.5MPa, microwave irradiation time 90min.
4, the microwave depolymerization method of polyethylene terephthalate according to claim 1 is characterized in that: 230 ℃ of temperature of reaction, reaction pressure 2.3MPa, microwave irradiation time 60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100254964A CN1239461C (en) | 2004-06-17 | 2004-06-17 | Microwave depolymerization method for PET |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100254964A CN1239461C (en) | 2004-06-17 | 2004-06-17 | Microwave depolymerization method for PET |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1594268A CN1594268A (en) | 2005-03-16 |
| CN1239461C true CN1239461C (en) | 2006-02-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100254964A Expired - Fee Related CN1239461C (en) | 2004-06-17 | 2004-06-17 | Microwave depolymerization method for PET |
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| Country | Link |
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| CN (1) | CN1239461C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ2007469A3 (en) * | 2007-07-13 | 2008-12-29 | Ústav chemických procesu Akademie ved CR | Method of waste polyethyleneterephthalate chemical depolymerization |
| CN101851326B (en) * | 2010-05-26 | 2013-09-25 | 华南理工大学 | Polyurethane elastomer and preparation method thereof |
| CN104458994B (en) * | 2014-12-16 | 2016-01-27 | 上海微谱化工技术服务有限公司 | The analytical approach of acryl resin |
| CN104892422B (en) * | 2015-05-05 | 2017-06-13 | 芜湖职业技术学院 | The biodegrading process of polyester fiber |
| CN104878598B (en) * | 2015-06-11 | 2017-07-14 | 中原工学院 | A kind of microwave radiation technology ammonolysis method of surface hydrophilic terylene |
| CN106149092B (en) * | 2016-07-15 | 2019-01-01 | 安徽双帆高纤有限公司 | Recycled polyester material flexibility preparation process |
| CZ2018120A3 (en) * | 2018-03-12 | 2019-04-10 | JBPV s.r.o. | A method of producing terephthalic acid from waste polyethylene terephthalate |
| CN110344128B (en) * | 2019-07-17 | 2021-04-13 | 军事科学院***工程研究院军需工程技术研究所 | Preparation method of microporous linen-like fiber |
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2004
- 2004-06-17 CN CNB2004100254964A patent/CN1239461C/en not_active Expired - Fee Related
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