WO2001021373A1 - Procede de preparation de resine polyethylene terephthalate apte au contact alimentaire a partir de recipients pet jetables - Google Patents

Procede de preparation de resine polyethylene terephthalate apte au contact alimentaire a partir de recipients pet jetables Download PDF

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Publication number
WO2001021373A1
WO2001021373A1 PCT/AU2000/001131 AU0001131W WO0121373A1 WO 2001021373 A1 WO2001021373 A1 WO 2001021373A1 AU 0001131 W AU0001131 W AU 0001131W WO 0121373 A1 WO0121373 A1 WO 0121373A1
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WO
WIPO (PCT)
Prior art keywords
pet
flakes
process according
materials
millibar
Prior art date
Application number
PCT/AU2000/001131
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English (en)
Inventor
Edward Kosior
Original Assignee
Visy Plastics Pty Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Visy Plastics Pty Ltd filed Critical Visy Plastics Pty Ltd
Priority to EP00965627A priority Critical patent/EP1244540A4/fr
Priority to BR0014094-5A priority patent/BR0014094A/pt
Priority to NZ517832A priority patent/NZ517832A/en
Priority to CA002384878A priority patent/CA2384878A1/fr
Priority to JP2001524779A priority patent/JP2003509249A/ja
Priority to AU76310/00A priority patent/AU777435C/en
Priority to KR1020027003540A priority patent/KR20020055580A/ko
Publication of WO2001021373A1 publication Critical patent/WO2001021373A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04—Disintegrating plastics, e.g. by milling
    • B29B17/0412—Disintegrating plastics, e.g. by milling to large particles, e.g. beads, granules, flakes, slices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B2013/002—Extracting undesirable residual components, e.g. solvents, unreacted monomers, from material to be moulded
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B13/00—Conditioning or physical treatment of the material to be shaped
    • B29B2013/005—Degassing undesirable residual components, e.g. gases, unreacted monomers, from material to be moulded
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • B29B2017/0203—Separating plastics from plastics
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • B29B2017/0213—Specific separating techniques
    • B29B2017/0286—Cleaning means used for separation
    • B29B2017/0289—Washing the materials in liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/02—Separating plastics from other materials
    • B29B2017/0213—Specific separating techniques
    • B29B2017/0293—Dissolving the materials in gases or liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
    • B29K2067/003—PET, i.e. poylethylene terephthalate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
    • B29K2105/065—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts containing impurities
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
    • B29K2105/26—Scrap or recycled material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/712—Containers; Packaging elements or accessories, Packages
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/712—Containers; Packaging elements or accessories, Packages
    • B29L2031/7158—Bottles
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock
    • Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics
    • 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

Definitions

  • This invention relates to methods for preparing polyethylene terephthalate (PET) resin from plastic waste that includes PET containers. It also relates to PET obtained according to the process.
  • PET polyethylene terephthalate
  • PET is a widely used polymer or resin with a broad range of applications but which has a particularly widespread use as a beverage container or bottle.
  • the use of PET for beverage containers has increased rapidly over the last decade and has to a large extent replaced conventional glass beverage containers especially for carbonated soft drinks.
  • Part of the widespread acceptance of PET has been attributed to its ability to be used for food contact as well as its light weight relative to glass of comparable strength and its ability to resist breakage.
  • PET containers most of the applications for recycled PET are for relatively low specification products that use a mixture of thermoplastic resins or polymers including PET. In these applications removal of contaminants is not important. It is desirable that PET containers may be recycled to produce PET resin that is suitable for the same applications as virgin PET. For example, it is especially desirable that the recycled resin may be used for food contact applications. However, for such applications there are strict limits on the presence of contaminants.
  • a further approach to recycling PET for food grade applications is disclosed in Australian Patent Application No. 9478299.
  • beverage containers are produced having inner and outer skins.
  • the inner skin which is in contact with food is made from virgin PET and the outer skin is made from recycled PET resin.
  • This invention removes the necessity for the recycled PET being suitable for food contact.
  • recycled PET can be used for direct food applications without using multiple skin production methods with their associated complexities and costs.
  • PET originating from sorted collections of solid urban refuse can be contaminated with a range of materials. These include other polymers especially polyolefins such as HDPE. Other common contaminants are metals, particulate material such as dirt, glues, paper, inks and remnants of materials stored in the containers. It is desirable that food contact grade PET may be obtained from such collections of urban refuse. Summary of the Invention
  • This invention provides in one form a process for preparing food contact grade PET from a waste stream containing PET and non PET materials comprising the following steps: sorting at least some of the non PET materials from the waste stream; dividing the PET containers into flakes of preferable maximum size approximately 10mm; washing the flakes in a hot aqueous medium containing alkaline materials and surfactants, preferably non-ionic, to remove particulate and absorbed contaminants from the surfaces of the flakes; de- watering and then drying the flakes to a moisture content of 0.1% w/w maximum, and more preferably 0.01 % w/w maximum; optionally removing absorbed contaminants and moisture by heating and vigorously mixing the flakes under vacuum, preferably 1- 10 millibar, more preferably 2 - 7 millibar and at a temperature less than the melting point of PET, preferably in the range 170-220°C for at least 30 minutes, preferably at least 60 minutes; melting the flakes in a screw extruder under vacuum to remove absorbed contaminant and; extruding
  • the material in the extruder is maintained at 280 - 290°C with a residence time of less than 60 seconds.
  • the heating to remove the absorbed contaminants is attained by frictional forces from the vigorous mixing.
  • the recycled PET must have contamination sufficiently low than such that the level of extractables is less than 10 ppb.
  • a range of materials may be adsorbed into or absorbed onto PET surfaces. These contaminants can include organo metallic materials such as copper octoate. Absorbed materials may include polar and non polar organic materials that have a range of volatilities.
  • An urban solid waste stream consisting of baled bottles are passed through a debaler that singulates the bottles so that they can be fed at a steady rate to the inlet of a pre-wash unit.
  • the preferred pre-wash unit is a Sorema Bottle Pre-wash unit that utilises elevated temperatures and alkaline surfactants.
  • similar units that have either a continuous or batch-wise mode of operation may also be used.
  • the feed rate is typically in the range 500 kgs to 2500 kgs per hour with 1500 kgs per hour being the optimum rate.
  • the action of the pre-wash unit is to tumble the bottles using the rotary motion of the cylindrical tumbler unit about its longitudinal axis. Internal baffles in the tumbler ensure that all bottles are singulated by repeated impact of the bottles falling against the walls and baffles while they are exposed to hot water and steam.
  • the internal temperature is typically maintained in the range 90 to 100°C with temperatures greater than 95°C being preferred.
  • the residence time in the pre-wash unit is generally in the range between 3 minutes and 15 minutes with a typical time being 5 minutes.
  • the water in the pre-wash may include cleaning agents such as caustic soda and non-foaming detergents. Typical concentrations of the caustic soda and detergent are 0.1 to 3% (ideally 0.5%) and 0.1 to 0.5% (ideally 0.2%) respectively.
  • the preferred detergent or surfactant is non-ionic.
  • the wash bottles are then de-watered by tumbling them in a cylindrical tumbler or similar device that allows the freed dirt and other contaminants such as labels and closures to pass through the perforations in the walls of the tumbler.
  • the water can be reused after it is filtered and treated to remove foreign materials.
  • the residence time in this de- watering unit is in the range 3 minutes and 15 minutes with a typical time being 5 minutes.
  • bottles are clean externally except for a film of water and are mostly free of plastic or paper labels through the action of the mechanical handling of the bottles, the hot water and the cleaning agents.
  • the PET bottles are then sorted.
  • the preferred process uses automatic systems such as those made by MSS, ROFIN or NRT although manual sorting can also be used. Particularly good results are achieved when a sequence of MSS Binary modules are used to sort the PET bottles to give a level of purity of no more than 20 ppm of PVC.
  • the level of sorting of non PET should be to 99.998% purity.
  • the MSS modules use modular sensors to detect the presence of specific plastics and air jets to eject the bottles at a specific station.
  • the first module uses an X-ray absorption to detect the chlorine atom in PVC and the PVC bottles are ejected at this station. This module also removes aluminium cans due to their strong X-ray absorption.
  • the second module uses infra-red absorption to detect HDPE (high density polyethylene) bottles and these are then ejected.
  • HDPE high density polyethylene
  • the third module uses near infra-red absorption to detect PET and in this module all the non PET bottles are ejected.
  • This module will eject bottles such as PVC, HDPE, polypropylene, polystyrene and aluminium cans.
  • the fourth module uses X-ray absorption to detect the chlorine atom in PVC and the PVC bottles are ejected at this station. This module also removes aluminium cans due to their strong X-ray absorption.
  • a manual inspection is used to finally check that only PET bottles proceed into the later stages of the process.
  • the sorted PET containers are then reduced in size using a wet grinder such as a Sorema hot wash, separation and rinsing system or its equivalent.
  • a wet grinder such as a Sorema hot wash, separation and rinsing system or its equivalent.
  • the wet grinder uses multiple rotating knives to cut the PET bottles against stationary knives in the presence of water that is at ambient temperature or at elevated temperatures (from 10 to 40°C, with 15 to 20°C being most often used), and which will contain caustic soda and low foaming surfactants and antifoam additives.
  • Typical concentrations of the caustic soda and detergent is 0.1 to 3% (ideally 0.5%) and 0.1 to 0.5% (ideally 0.2%) respectively.
  • Anti-foam use is related to surfactant level and is usually in the range 0.01 to 1%.
  • the PET bottles are cut against a screen with a hole size of 10mm to 30mm with 16 to 20 mm being the most common. This gives an intense washing and simultaneous cutting effect on the PET bottles resulting in a range of average flake sizes that varies from 3mm to 12mm with the most numerous being under 8mm.
  • the mixture of PET flake and polypropylene particles is fed into Sorema Hot Wash Reactors (or similar) where the mix is intensively washed for 10 to 20 minutes at temperatures from 75 to 95°C with 90°C being the ideal.
  • the flakes are fed into the reactors at a liquid to plastic flake slurry ratio of 90/10 to 65/35 with 75/25 Volume/Volume being most common.
  • the reactors are designed to provide turbulent washing conditions where particles impinge on each other through the use of opposed-rotor, dual-rotor stirrers that are used in non-central positions to prevent laminar mixing from occurring, thus ensuring the most intense washing effect on the PET flakes.
  • the flakes After washing the flakes are separated from the wash solution by the use of a centifruge or screen, and the flakes are subjected to a sink-float separation in a tank of water where the polypropylene particles float due to their density being less than that of water (915 kg/m 3 ) and the PET particles sink due to their density being greater than that of water (1400 kg/m 3 ).
  • the separated PET flakes are then further rinsed at least twice in clean water to remove the residual traces of surfactants and dilute contaminants.
  • the pathway of the water and flakes is counter current to provide the maximum rising effect.
  • the PET flakes are then de-watered to give a very low level of moisture, i.e. down to 0.005% water.
  • the fluidised bed driers will remove the moisture from saturated levels down to levels of less than 1% and typically 0.5%.
  • the desiccant driers, Erema agglomerators or other driers will reduce the moisture level to at least 0.01% i.e. lOOOppm of water with an ideal level of 0.005% of moisture, i.e. 500ppm. In conventional driers this may require the use of long residence times as well as high temperatures, eg. temperatures of the order of 120 to 175°C for 8 to 5 hours with 170°C for 5 hours proving optimum.
  • the use of pre drying of the PET flakes is important as it leads to an increase rather than decrease in the intrinsic viscosity (IV) of the polymer in the following stages of the process. For example, the IV of the final PET pellet with the pre drying step was 0.833 versus 0.749 without compared to the IV of the flake itself of 0.767.
  • the dried flakes are then subjected to vacuum decontamination.
  • This process uses high levels of vacuum, preferably 1- 10 millibar, more preferably 2 - 7 millibar, while the PET is subjected to elevated temperatures (170 to 215°C) and mixing for controlled residence times of typically 1 hour, although longer times may also be useful.
  • This decontamination can be performed in an Erema shredder chamber modified to maintain a vacuum, or in a fluidising mixer modified to hold a vacuum. Frictional forces between flakes and parts of the equipment lead to heat build up and this is the preferred method of attaining the desired temperature.
  • the impeller in the chamber is rotated at between 200 to 220 rpm converting mechanical energy into heat. Increasing the speed generates high temperatures with typically a temperature gradient, the higher temperatures being at the bottom. For example, when the impeller speed was 220 rpm the temperature at the bottom was 199°C, in the middle was 189°C and at the top 169°C.
  • the loading of the chamber with the PET flakes and the rotor speed are selected so that the chamber was filled to a sufficiently high level, approximately 70%, that flake introduced through a vacuum lock could reside at the top for a controlled residence time without the risk of immediately being mixed into the bulk of the flake and being extruded with only a short residence time.
  • the conditions in the chamber were balanced so that the PET flake was progressively exposed to higher temperatures while under high vacuum and maintained at this condition for at least one hour after which it was introduced into the extruder.
  • the decontamination of the PET takes place in the mixer by the combined action of the vacuum, elevated temperature and the residence time of the PET under these conditions.
  • the decontaminated PET flakes are then fed to a screw extruder, such as an Erema extruder, with an extrusion screw designed for the processing of PET and capable of applying vacuum venting to the PET melt at 280 to 290°C.
  • a screw extruder such as an Erema extruder
  • the process could be conducted in a similar twin screw extruder with vacuum venting or in a twin or multi-screw extruder with vacuum venting.
  • the key requirement is the capability to melt the PET (melt temperature in the range 265 - 300°C, preferably 280°C) and to apply one or more stages of vacuum venting (at preferably 1 millibar or less) without applying excessive shear to the PET in the melt stage through excessive mechanical working of the melt. Excessive shear leads to a decrease in the IV.
  • the application of the higher temperatures in the melt coupled with the vacuum venting allows removal of the least volatile fluids that may have been absorbed into the PET.
  • Chain extender materials are known and usually comprise one or more of a polycarboxylic acid or anhydride, a polyol and an esterification catalyst.
  • a mixture of pyromellitic anhydride, pentaerythritol and antimony oxide in the weight ratios of 4: 1 :0.5 is a particularly useful chain extender composition.
  • this chain extender composition has been able to increase the IV of the PET to 0.930 when used at 0.3% w/w of PET. Higher levels, eg 1.0% w/w increased the IV to 1.300.
  • the melt After melting and vacuum venting the melt is filtered by passing it through fine metal mesh filters (usually the mesh size is 120 mesh or finer) to remove any particles.
  • fine metal mesh filters usually the mesh size is 120 mesh or finer
  • the extruded melt may then be converted to pellets typically 3mm using conventional techniques such as by using an underwater die face cutter or hot die face and water ring that quenches the melt into pellets as they are cut. Further steps may include crystallising the pellets and pre-drying the pellets prior to moulding. The crystallising is carried out by heating the PET pellets while they are kept moving via tumbling or agitation. The temperature is maintained at from 120°C to 170°C for between 10 minutes and 1 hour.
  • Pre drying is carried out by heating the pellets at elevated temperatures in hot gas that has a dew point of less than 40°C.
  • the temperatures used typically vary from 140°C to 190°C for a duration that typically varies from 4 hours to 7 hours.
  • the effectiveness of the recycling process of the present invention is illustrated by introducing the following contaminants to PET containers: toluene 10% v/v, chloroform 10% u/v, benzophenone 1% v/v, methyl stearate 1% v/v and copper octoate 1% v/v.
  • the concentrations of these contaminants after the various stages of the process steps of the present invention are set out in Table 1. These results show that after the process of the present invention contamination levels in the extruded pellets are acceptably low.
  • the Table also shows the levels of extractables from PET bottles made from pellets prepared as described above.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Sustainable Development (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

L'invention concerne un procédé de préparation de PET apte au contact alimentaire à partir d'un flux de déchets contenant des matières PET et non PET. Le procédé comprend les étapes consistant en un tri au moins certaines des matières non PET du flux de déchets, suivi d'une séparation des récipients PET en flocons d'une grosseur maximum préférable d'approximativement 10 mm, suivie d'un lavage des flocons dans un milieu aqueux chaud contenant des matières et des tensioactifs alcalins, de préférence non ioniques, afin d'éliminer les contaminants particulaires et absorbés des surfaces des flocons. Cette étape est suivie d'un égouttage et ensuite d'un séchage des flocons jusqu'à obtention d'une teneur en humidité de 0,1 % en poids au maximum, et de préférence de 0,01 % en poids au maximum. L'étape suivante consiste à éliminer les contaminants absorbés et l'humidité par chauffage et mélange vigoureux des flocons sous vide, de préférence à 1-10 millibars, idéalement à 2-7 millibars et à une température inférieure à la température du point de fusion du PET, de préférence dans la gamme 170-220 °C pendant au moins 30 minutes, de préférence au moins 60 minutes. L'étape finale consiste à faire fusionner les flocons dans une extrudeuse à vis équipée pour un traitement sous vide et à extruder la matière fusionnée pour former des brins qui sont pastillés.
PCT/AU2000/001131 1999-09-17 2000-09-18 Procede de preparation de resine polyethylene terephthalate apte au contact alimentaire a partir de recipients pet jetables WO2001021373A1 (fr)

Priority Applications (7)

Application Number Priority Date Filing Date Title
EP00965627A EP1244540A4 (fr) 1999-09-17 2000-09-18 Procede de preparation de resine polyethylene terephthalate apte au contact alimentaire a partir de recipients pet jetables
BR0014094-5A BR0014094A (pt) 1999-09-17 2000-09-18 Processo para preparar um poli (tereftalato de etileno) de tipo para contato com alimentos e poli (tereftalato de etileno) reciclado
NZ517832A NZ517832A (en) 1999-09-17 2000-09-18 Process for preparing food contact grade polyethylene terephthalate resin from waste pet containers
CA002384878A CA2384878A1 (fr) 1999-09-17 2000-09-18 Procede de preparation de resine polyethylene terephthalate apte au contact alimentaire a partir de recipients pet jetables
JP2001524779A JP2003509249A (ja) 1999-09-17 2000-09-18 廃ｐｅｔ容器から食品接触グレードポリエチレンテレフタレート樹脂を製造する方法
AU76310/00A AU777435C (en) 1999-09-17 2000-09-18 Process for preparing food contact grade polyethylene terephthalate resin from waste pet containers
KR1020027003540A KR20020055580A (ko) 1999-09-17 2000-09-18 폐기된 페트 용기로부터 식품 접촉 등급의 폴리에틸렌테레프탈레이트 수지를 제조하는 방법

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AUPQ2946A AUPQ294699A0 (en) 1999-09-17 1999-09-17 Process for preparing food contact grade polyethylene terephthalate resin from waste pet containers
AUPQ2946 1999-09-17

Publications (1)

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WO2001021373A1 true WO2001021373A1 (fr) 2001-03-29

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PCT/AU2000/001131 WO2001021373A1 (fr) 1999-09-17 2000-09-18 Procede de preparation de resine polyethylene terephthalate apte au contact alimentaire a partir de recipients pet jetables

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EP (1) EP1244540A4 (fr)
JP (1) JP2003509249A (fr)
KR (1) KR20020055580A (fr)
AU (2) AUPQ294699A0 (fr)
BR (1) BR0014094A (fr)
CA (1) CA2384878A1 (fr)
NZ (1) NZ517832A (fr)
WO (1) WO2001021373A1 (fr)

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DE10054226A1 (de) * 2000-11-02 2002-05-08 Buehler Ag Verfahren zur Verarbeitung eines Polykondensats in einem Mehrwellen-Extruder
DE10032900C2 (de) * 2000-07-06 2002-11-21 B & B Anlagenbau Gmbh Verfahren zum Aufbereiten von PET-Behältnissen mit einer alkalischen Hydrolyse
US6984694B2 (en) 2002-02-01 2006-01-10 Johnson Polymer, Llc Oligomeric chain extenders for processing, post-processing and recycling of condensation polymers, synthesis, compositions and applications
US7297721B2 (en) 2003-06-20 2007-11-20 Futura Polyesters Limited Process for controlled polymerization of a mixed polymer
WO2008017843A1 (fr) * 2006-08-09 2008-02-14 The Waste And Resources Action Programme Procédé de recyclage du poly (téréphthalate d'éthylène) (pet)
US7973092B2 (en) 2003-10-13 2011-07-05 Krones Ag PET bottle recycling
EP2365018A1 (fr) * 2010-03-09 2011-09-14 Nakamoto Packs Co., Ltd. Procédé de fabrication de feuille pour récipients d'aliments
WO2013019868A1 (fr) * 2011-08-02 2013-02-07 Mba Polymers, Inc. Procédés de réduction de la contamination dans des plastiques récupérés de de biens durables
US8394866B2 (en) 2005-03-24 2013-03-12 Krones Ag Method and device for the decontamination of plastic flakes
WO2013151640A2 (fr) 2012-04-03 2013-10-10 Macdermid Acumen, Inc. Additif à utiliser dans l'étape de lavage de processus de recyclage de polyéthylène téréphtalate
EP2720841A2 (fr) * 2011-06-20 2014-04-23 Essel Propack Limited Procédé de recyclage de plastiques, produits et applications associés
US9028943B2 (en) 2012-10-30 2015-05-12 Mba Polymers, Inc. Method for improving the surface appearance and processing of plastics recovered from durable goods
WO2016005493A1 (fr) * 2014-07-10 2016-01-14 Nestec S.A. Procédé de traitement de téréphtalate de polyéthylène
WO2016081568A1 (fr) * 2014-11-18 2016-05-26 Mohawk Industries, Inc. Systèmes et procédés de fabrication de filament continu gonflant
US9550338B2 (en) 2012-05-31 2017-01-24 Mohawk Industries, Inc. Systems and methods for manufacturing bulked continuous filament
US9630353B2 (en) 2012-05-31 2017-04-25 Mohawk Industries, Inc. Method of manufacturing bulked continuous filament
US9630354B2 (en) 2012-05-31 2017-04-25 Mohawk Industries, Inc. Method of manufacturing bulked continuous filament
US9636845B2 (en) 2012-05-31 2017-05-02 Mohawk Industries, Inc. Method of manufacturing pet nurdles
US9636860B2 (en) 2012-05-31 2017-05-02 Mohawk Industries, Inc. Method of manufacturing bulked continuous filament
ITUB20155870A1 (it) * 2015-11-25 2017-05-25 Previero Sas Metodo ed apparato per il dosaggio di una o piu' sostanze per il trattamento di materie plastiche
WO2018127431A1 (fr) * 2017-01-03 2018-07-12 Alpla Werke Alwin Lehner Gmbh & Co. Kg Regranulé de pet à viscosité intrinsèque élevée et son procédé de fabrication
US20190118413A1 (en) 2012-05-31 2019-04-25 Mohawk Industries, Inc. Systems and methods for manufacturing bulked continuous filament from colored recycled pet
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US10751915B2 (en) 2016-11-10 2020-08-25 Aladdin Manufacturing Corporation Polyethylene terephthalate coloring systems and methods
US11045979B2 (en) 2012-05-31 2021-06-29 Aladdin Manufacturing Corporation Methods for manufacturing bulked continuous filament from recycled PET
WO2021185757A1 (fr) * 2020-03-16 2021-09-23 Alpla Werke Alwin Lehner Gmbh & Co. Kg Procédé de préparation d'une matière de départ pet convenant pour la mise en œuvre d'un procédé d'extrusion-soufflage et corps creux réalisé au moyen du procédé d'extrusion-soufflage
US11242622B2 (en) 2018-07-20 2022-02-08 Aladdin Manufacturing Corporation Bulked continuous carpet filament manufacturing from polytrimethylene terephthalate
US11279071B2 (en) 2017-03-03 2022-03-22 Aladdin Manufacturing Corporation Method of manufacturing bulked continuous carpet filament
US11351747B2 (en) 2017-01-30 2022-06-07 Aladdin Manufacturing Corporation Systems and methods for manufacturing bulked continuous filament from colored recycled PET
US11473216B2 (en) 2017-09-15 2022-10-18 Aladdin Manufacturing Corporation Polyethylene terephthalate coloring systems and methods
WO2023203148A1 (fr) * 2022-04-22 2023-10-26 Alpla Werke Alwin Lehner Gmbh & Co. Kg Procédé de recyclage de récipients en polyester

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KR101301555B1 (ko) * 2013-03-07 2013-09-06 박철우 폴리에틸렌 파이프 제조용 재생원료 가공방법
DE102018009171A1 (de) * 2018-11-22 2020-05-28 Bb Engineering Gmbh Verfahren und Vorrichtung zum Recyceln von Kunststoffen
TWI761195B (zh) * 2021-04-29 2022-04-11 南亞塑膠工業股份有限公司 由回收膜形成聚酯材的方法
JP7185366B1 (ja) 2022-06-23 2022-12-07 株式会社日本選別化工 ペットボトルの異物除去方法及び異物除去装置

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DE10032900C2 (de) * 2000-07-06 2002-11-21 B & B Anlagenbau Gmbh Verfahren zum Aufbereiten von PET-Behältnissen mit einer alkalischen Hydrolyse
DE10054226A1 (de) * 2000-11-02 2002-05-08 Buehler Ag Verfahren zur Verarbeitung eines Polykondensats in einem Mehrwellen-Extruder
US6984694B2 (en) 2002-02-01 2006-01-10 Johnson Polymer, Llc Oligomeric chain extenders for processing, post-processing and recycling of condensation polymers, synthesis, compositions and applications
US7297721B2 (en) 2003-06-20 2007-11-20 Futura Polyesters Limited Process for controlled polymerization of a mixed polymer
US7973092B2 (en) 2003-10-13 2011-07-05 Krones Ag PET bottle recycling
US8394866B2 (en) 2005-03-24 2013-03-12 Krones Ag Method and device for the decontamination of plastic flakes
EP1861455B2 (fr) † 2005-03-24 2015-07-29 Krones AG Procede et dispositif pour decontaminer des paillettes de plastique
US8557882B2 (en) 2005-03-24 2013-10-15 Krones Ag Method and device for the decontamination of plastic flakes
WO2008017843A1 (fr) * 2006-08-09 2008-02-14 The Waste And Resources Action Programme Procédé de recyclage du poly (téréphthalate d'éthylène) (pet)
US8470224B2 (en) 2010-03-09 2013-06-25 Nakamoto Packs Co., Ltd. Method of manufacturing sheet for food containers
EP2365018A1 (fr) * 2010-03-09 2011-09-14 Nakamoto Packs Co., Ltd. Procédé de fabrication de feuille pour récipients d'aliments
EP2720841A2 (fr) * 2011-06-20 2014-04-23 Essel Propack Limited Procédé de recyclage de plastiques, produits et applications associés
EP2720841A4 (fr) * 2011-06-20 2015-04-29 Essel Propack Ltd Procédé de recyclage de plastiques, produits et applications associés
WO2013019868A1 (fr) * 2011-08-02 2013-02-07 Mba Polymers, Inc. Procédés de réduction de la contamination dans des plastiques récupérés de de biens durables
US9359482B2 (en) 2011-08-02 2016-06-07 Mba Polymers, Inc. Methods for reducing contamination in plastics recovered from durable goods
WO2013151640A2 (fr) 2012-04-03 2013-10-10 Macdermid Acumen, Inc. Additif à utiliser dans l'étape de lavage de processus de recyclage de polyéthylène téréphtalate
US9636845B2 (en) 2012-05-31 2017-05-02 Mohawk Industries, Inc. Method of manufacturing pet nurdles
US10239247B2 (en) 2012-05-31 2019-03-26 Mohawk Industries, Inc. Methods for manufacturing bulked continuous filament
US11007673B2 (en) 2012-05-31 2021-05-18 Aladdin Manufacturing Corporation Methods for manufacturing bulked continuous filament from colored recycled PET
US9550338B2 (en) 2012-05-31 2017-01-24 Mohawk Industries, Inc. Systems and methods for manufacturing bulked continuous filament
US9630353B2 (en) 2012-05-31 2017-04-25 Mohawk Industries, Inc. Method of manufacturing bulked continuous filament
US9630354B2 (en) 2012-05-31 2017-04-25 Mohawk Industries, Inc. Method of manufacturing bulked continuous filament
US11045979B2 (en) 2012-05-31 2021-06-29 Aladdin Manufacturing Corporation Methods for manufacturing bulked continuous filament from recycled PET
US9636860B2 (en) 2012-05-31 2017-05-02 Mohawk Industries, Inc. Method of manufacturing bulked continuous filament
US11780145B2 (en) 2012-05-31 2023-10-10 Aladdin Manufacturing Corporation Method for manufacturing recycled polymer
US11724418B2 (en) 2012-05-31 2023-08-15 Aladdin Manufacturing Corporation Methods for manufacturing bulked continuous carpet filament
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US10124513B2 (en) 2012-05-31 2018-11-13 Mohawk Industries, Inc. Methods for manufacturing bulked continuous filament
US10232542B2 (en) 2012-05-31 2019-03-19 Mohawk Industries, Inc. Methods for manufacturing bulked continuous filament
US11911930B2 (en) 2012-05-31 2024-02-27 Aladdin Manufacturing Corporation Methods for manufacturing bulked continuous filament from recycled PET
US20190118413A1 (en) 2012-05-31 2019-04-25 Mohawk Industries, Inc. Systems and methods for manufacturing bulked continuous filament from colored recycled pet
US11273579B2 (en) 2012-05-31 2022-03-15 Aladdin Manufacturing Corporation Systems and methods for manufacturing bulked continuous filament
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US10744681B2 (en) 2012-05-31 2020-08-18 Aladdin Manufacturing Corporation Methods for manufacturing bulked continuous filament
US11179868B2 (en) 2012-05-31 2021-11-23 Aladdin Manufacturing Corporation Systems and methods for manufacturing bulked continuous filament
US9028943B2 (en) 2012-10-30 2015-05-12 Mba Polymers, Inc. Method for improving the surface appearance and processing of plastics recovered from durable goods
WO2016005493A1 (fr) * 2014-07-10 2016-01-14 Nestec S.A. Procédé de traitement de téréphtalate de polyéthylène
US10343323B2 (en) 2014-07-10 2019-07-09 Nestec S.A. Method for processing polyethylene terephthalate
WO2016081568A1 (fr) * 2014-11-18 2016-05-26 Mohawk Industries, Inc. Systèmes et procédés de fabrication de filament continu gonflant
CN108350208A (zh) * 2015-11-25 2018-07-31 普瑞威努公司 用于在用于洗涤和回收塑料的系统中定量给料一种或多种处理物质的方法
CN108350208B (zh) * 2015-11-25 2021-12-21 普瑞威努公司 用于在用于洗涤和回收塑料的系统中定量给料一种或多种处理物质的方法
ITUB20155870A1 (it) * 2015-11-25 2017-05-25 Previero Sas Metodo ed apparato per il dosaggio di una o piu' sostanze per il trattamento di materie plastiche
WO2017089883A1 (fr) * 2015-11-25 2017-06-01 Previero N. S.R.L. Procédé de dosage d'une ou plusieurs substances de traitement dans un système de lavage et de recyclage de plastiques
US10751915B2 (en) 2016-11-10 2020-08-25 Aladdin Manufacturing Corporation Polyethylene terephthalate coloring systems and methods
US11254797B2 (en) 2017-01-03 2022-02-22 Alpla Werke Alwin Lehner Gmbh & Co. Kg Pet regranulate having high intrinsic viscosity and method for the production thereof
CH713339A1 (de) * 2017-01-03 2018-07-13 Alpla Werke Alwin Lehner Gmbh & Co Kg PET-Regranulat mit hoher intrinsischer Viskosität und Verfahren zu dessen Herstellung.
WO2018127431A1 (fr) * 2017-01-03 2018-07-12 Alpla Werke Alwin Lehner Gmbh & Co. Kg Regranulé de pet à viscosité intrinsèque élevée et son procédé de fabrication
US11840039B2 (en) 2017-01-30 2023-12-12 Aladdin Manufacturing Corporation Systems and methods for manufacturing bulked continuous filament from colored recycled PET
US11351747B2 (en) 2017-01-30 2022-06-07 Aladdin Manufacturing Corporation Systems and methods for manufacturing bulked continuous filament from colored recycled PET
US11279071B2 (en) 2017-03-03 2022-03-22 Aladdin Manufacturing Corporation Method of manufacturing bulked continuous carpet filament
US11473216B2 (en) 2017-09-15 2022-10-18 Aladdin Manufacturing Corporation Polyethylene terephthalate coloring systems and methods
US11618973B2 (en) 2017-09-15 2023-04-04 Aladdin Manufacturing Corporation Polyethylene terephthalate coloring systems and methods
US11242622B2 (en) 2018-07-20 2022-02-08 Aladdin Manufacturing Corporation Bulked continuous carpet filament manufacturing from polytrimethylene terephthalate
US11926930B2 (en) 2018-07-20 2024-03-12 Aladdin Manufacturing Corporation Bulked continuous carpet filament manufacturing from polytrimethylene terephthalate
WO2021185757A1 (fr) * 2020-03-16 2021-09-23 Alpla Werke Alwin Lehner Gmbh & Co. Kg Procédé de préparation d'une matière de départ pet convenant pour la mise en œuvre d'un procédé d'extrusion-soufflage et corps creux réalisé au moyen du procédé d'extrusion-soufflage
CH717234A1 (de) * 2020-03-16 2021-09-30 Alpla Werke Alwin Lehner Gmbh & Co Kg Verfahren zur Herstellung eines zur Verwendung in einem Extrusionsblasverfahren geeigneten PET-Ausgangsmaterials und daraus hergestellter Hohlkörper.
CH719619A1 (de) * 2022-04-22 2023-10-31 Alpla Werke Alwin Lehner Gmbh & Co Kg Verfahren zum Recycling von Polyester-Behältern.
WO2023203148A1 (fr) * 2022-04-22 2023-10-26 Alpla Werke Alwin Lehner Gmbh & Co. Kg Procédé de recyclage de récipients en polyester

Also Published As

Publication number Publication date
KR20020055580A (ko) 2002-07-09
NZ517832A (en) 2002-06-28
BR0014094A (pt) 2002-05-21
EP1244540A4 (fr) 2002-11-06
EP1244540A1 (fr) 2002-10-02
AU7631000A (en) 2001-04-24
AUPQ294699A0 (en) 1999-10-14
JP2003509249A (ja) 2003-03-11
AU777435C (en) 2006-02-23
CA2384878A1 (fr) 2001-03-29
AU777435B2 (en) 2004-10-14

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