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WO1994009064A1 - Procede de recuperation de polythene et de polypropylene et autres polyolefines a partir de materiaux de retour, notamment ceux de type composite - Google Patents

Procede de recuperation de polythene et de polypropylene et autres polyolefines a partir de materiaux de retour, notamment ceux de type composite Download PDF

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Publication number
WO1994009064A1
WO1994009064A1 PCT/SE1993/000836 SE9300836W WO9409064A1 WO 1994009064 A1 WO1994009064 A1 WO 1994009064A1 SE 9300836 W SE9300836 W SE 9300836W WO 9409064 A1 WO9409064 A1 WO 9409064A1
Authority
WO
WIPO (PCT)
Prior art keywords
polyolefine
solvent
solution
water
polyolefines
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/SE1993/000836
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English (en)
Inventor
Sven Ljungbo
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
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
Priority claimed from SE9203027A external-priority patent/SE470212B/sv
Application filed by Individual filed Critical Individual
Publication of WO1994009064A1 publication Critical patent/WO1994009064A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
    • C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
    • 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
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • 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
    • 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
    • Y02W30/80—Packaging reuse or recycling, e.g. of multilayer packaging

Definitions

  • the present invention is a method to regain polythene, polyprophylene and other polyolefines from return material such as production waste, assorted refuse, household garbage etc., in order to re-use them to the same or just as qualified products as by their first use.
  • the invention is founded upon the following qualities in polyolefines: PE and PP and many other polyolefines and some copolymers of olefines mutually combined or combined with other monomers are, at higher temperatures, soluble in several solvents, first hydro-carbons and chlorinated hydro-carbons. At rising percentage of the comonomer the temperature, required for disolving the polymer sinks and drops to room temperature or lower at higher comonomer proportions.
  • the temperature, at which a certain solvent dissolves a certain one of these polymeres, is thus different for different polymeres.
  • This temperature is below called the dissolving temperature.
  • polyolefines are characterized by their precipita- ting from the solvent as powder if the temperature of the solution is lowered under the dissolving temperature. Through pressfiltering this powder can be separated from the bulk of the solvent in the form of a powder cake, that can be rid of remaining solvents through drying.
  • the method proposed here is composed of the follo- wing elements:
  • the return material is if needed removed from other materials than paper and plastic products. Then it is mixed with solvent and heated to at least dissolving temperature so as to dissolve the polyolefine in the material. The solution and the remaining not dissolved material are separated whereupon the restmaterial is washed a couple of times with a new solvent at the same temperature, alternatively washed once with counter flow. If the return material has such qualities that already the first dissolution of the polymer can be made by solvent flowing through without the bulk getting sticky and corking up the apparatures the whole dissolving- and washing - process is carried through in one step by the counterflow principle.
  • the polyolefine solution segregated from the restmaterial, is then separated in polyolefine and solvent through chilling the solution to a temperature below dissolving temperature. Then the solution congeals into a powder bulk, rather jelly- like in the beginning.
  • the main part of the solvent can be removed through filtering i.e. through suction, centrifugalizing or pressfiltering.
  • the last part of the solvent is removed by evaporation. This is best done at temperatures so far below the dissolving temperature as possible; thus the dry polyolefine is produced in the form of a free- flowing powder. If the drying is done only a few dozen degrees below dissolving temperature the powder will sinter into a compact body, from which it may even be difficult to get out the last remains of the solvent.
  • the cooling of the warm polyolefine solution for precipitation of the polyolefine involves certain problems.
  • the precipitated polyolefine strives to form deposits on the tube walls in an ordinary heat exchanger and thus impairs the heat conduction. In the worst case the heat exchanges gets blocked up.
  • this problem is solved by leading the separated warm solution to a tank, where it is vacuum-destilled, the outgoing stream is chilled and condensed and the cold condensate returned to the tank.
  • the vacuum evapori- sation as well as the return of the cold condensate chills the solution, remaining in the tank, so the polyolefine is precipitated. This process is, however, both apparatus- energy-intensive, and, more over, difficult to make continuous.
  • the warm polyolefine solution is injected into a tank with cold water through a heat- insulated jet. Since the polyolefine as well as the solvent are insoluble in water the solution rises to the water surface, if the solvent is a hydrocarbon or sinks to the bottom, if the solvent is a chlorinated hydro carbon. When passing through the water the solution is chilled to about the same temperature as the water has. From the tank the solution is transported to the filter works, where the polyolefine is separated from the main part of the solvent, which is brought back to the start of the process to dissolve new return material. The water in the tank is chilled in a heat-exchanger or through jacket-cooling. Alternatively to this process the cold water can be injected or dropped into the polyolefine solution and the two liquids separated as described above. 2
  • the concentration 1 of these in the solvent regained at filtering must be kept below the level, that can give 2 unwished effects on the polyolefine, regained in the next set. This is best achieved 3 through continuous purification of a part of a solvent regained at the filtering from 4 these substances before it is returned to the process. The purification can be made 5 through distilling, membranefiltering or other methods. 6 7 When the return material partly or largely consists of polyolefine laminate with paper, 8 cardboard or other products of woodfibre, the polyolefine can of course be extracted 9 from these ones in the same way as mentioned above.
  • Example 1 Waste of production of a foil-laminate of PE and PP glued together with fuse glue, is decomposed into small pieces with a hammer-mill or a screwmill. Stirring them these pieces are leached with fivefold the amount of toluene so as to dissolve the fuse glue. Then the solution is separated from the foil residue. This residue is washed with pure toluene, separated from it and dried from remaining toluene.
  • This drying can be made by blowing steam at 1 ata through the residue and then condensing the water and toluene steams or through vacuum evaporation of the toluene, followed by its condensation.
  • the fuse glue can be dissolved by benzene, methylethylpentone, chloroform, dichloromethane and other solvents, which are easier to evaporate from the foil residue, due to their low boiling point.
  • the residue is mixed with its sevenfold amount of heptane and is heated and stirred in autoclave up to 110° c temperature and a pressure of 130-150 k Pa. Then the PE foil turns into solution which is separated from the undissolved PP foil.
  • the foil is washed at the same temperature with pure heptane, which , after separation, is used for dissolving the next lot.
  • the PE solution is chilled to 20° c temperature so as to precipitate the polythene.
  • the heptane is, as far as possible, centrifugalized away, whereupon the PE powdermass with the last heptane residue is spread out on a warm roll, which then boils away the heptane at 95 - 99° c.
  • the heptane steam is condensed in a cooler and brought back to the process.
  • the polythene appears as a porous sintered cake. If PE is wanted as powder, the drying ought to be carried out under vacuum at a temperature of below 30° c.
  • the heptane can be exchanged for hexane or pentane or iso-pentane (their boiling points at 1 ata is 68, 36 respectively 28° c).
  • the pressure at the dissolving process must be raised to about 400 k Pa for hexane and still higher for pentane and iso-pentane.
  • An alternative to the process described above is to treat the decomposed PE PP laminate with 105° c warm toluene, which then dissolves both the polythene and the fuse glue. After the separation of the solution from the PP foil pieces, the former is chilled to 20° c temperature, allowing PE to precipitate and be separated from the solution.
  • Example 2 Assorted milkpacks of twofold PE laminated cardboard are decomposed in a screwmill, then cleaned from possible scraps of glas, china, metal etc. and dispersed in water, 80 - 90° c temperature. To the water sodium hydroxide has been added in quantities of 1-2 % of the weight of the cardboard laminate.
  • the 3% paper- plastic-dispersion is strongly stirred during 5 minutes, after which the water is sucked out on a filterdrum, where the pulp also is cleaned from remaining lyewater, containing fat and casein rests dispersed by the lye.
  • the so washed pulp is dehydrated to a 10%-dryness and taken over to an autoclave. There it is mixed, strongly stirring it, with heptane in a quantity corresponding to 8 - 10 times the weight of the PE in the cardboard pulp.
  • the temperature is raised to 110° c. After 10 minutes' treatment at this temperature the stirring is stopped and the so formed heptane-solution separated the suspension through sedimentation, that is accelerated by vibration.
  • the so formed foil is taken up and dried on a warm 10 conveyor belt of for example steel band or woven wire, coated by teflon or silicone ⁇ rubber or another polymer with good releasing power against PE.
  • the PE foil
  • the coating of the cardboard, paper or conveyor belt can also be made by spreading 2 the solution with a knife or a guardboard. Usually it is then necessary to work with a 3 more diluted solution than coating made by injection-moulding and slit nozzle. 4 5
  • the process in example 3 and 4 means that the last stage in the recovery of the 6 polythene at the same time is the first, respectively one of the first, stages of process 7 in the recycling of the same PE. This gives a saving of one of the process steps, 8 compared to the methods in example 1 and 2 to reclaim PE, including the following 9 preparations of products made from it.
  • Example 5 If the return material contains printing ink or other matter, which at dissolving 4 temperatures for polythene is soluble in the solvent used for PE recycling for 5 example heptane it is made in the following way: 6 7 The washed paper plastic dispersion, described in example 2, with a dry content of 8 2-3 % and a temperature below the dissolving temperature of the polythene, best 9 done at 70-80° c , is mixed, stirring it all the time, with an amount of heptane, 0 corresponding to 1-3% of the weight of the dispersion. After 3-5 minutes i stirring the solvent is separated through sedimentation or centrifugalizing.
  • the 2 solvent has now dissolved or gelatined and turned absorbed in the printing ink film 3 on the inside of the external PE film of the cardboard laminate.
  • destination 4 the heptane is separated from the colour remains and restored to the process.
  • the dispersion, filtered from colour is drained to 10% dry content and further treated as in ex 2 or 3 or 4.
  • Such an example is the remains after sugar- rizing the cellulose and hemicellulose from household and building refuse - through for example highly concentrated hydrocloric acid - and the separation of the sugar for ethanol fermentation. These remains - mostly plastics and lignine powder - are treated in the same way as the one in the examples above.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

Il existe des procédés connus pour récupérer le polythène et le polypropène et autres polyoléfines à partir de matériaux de retour grâce à l'extraction au moyen de différents solvants, à des températures élevées, et à la précipitation de polyoléfines, hors de la solution, en abaissant la température. Le refroidissement de la solution est toutefois difficile à réaliser lorsque la polyoléfine précipitée est salie et produit des écoulements et des obstructions dans un échangeur de chaleur ordinaire. La présente invention résout ce problème en utilisant des solvants insolubles dans l'eau pour l'extraction, et en injectant la solution chaude dans de l'eau froide. Lorsque la densité de la solution diffère considérablement de celle de l'eau, soit la solution remonte à la surface de l'eau, soit elle tombe au fond du réservoir d'eau. Là, la dispersion des polyoléfines, formée lors du refroidissement, est séparée de l'eau et ensuite décomposée en solvants et un gâteau de filtre. Le gâteau de filtre est séparé par évaporation pour être transformé soit en une poudre, soit en un gâteau fritté de polyoléfine pure. Ou bien, le gâteau fritté peut également être chauffé à nouveau de manière à produire une nouvelle solution, mais considérablement plus concentrée que la première. La nouvelle solution est ensuite étalée ou pulvérisée sur une ligne de carton ou papier chauffé, après quoi le reste du solvant est vaporisé dans un espace fermé, avec récupération du solvant vaporisé. On obtient donc un stratifié-papier-polyoléfine qui peut être utilisé pour des emballages et autres. De la même façon, on peut obtenir un film-polyoléfine si la ligne - par exemple une ligne de fil ou bande d'acier - est revêtue de Téflon TM. Dans ce cas, le film, formé après évaporation de la solution, peut être retiré de la ligne et enroulé.
PCT/SE1993/000836 1992-10-15 1993-10-13 Procede de recuperation de polythene et de polypropylene et autres polyolefines a partir de materiaux de retour, notamment ceux de type composite Ceased WO1994009064A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE9203027A SE470212B (sv) 1992-08-25 1992-10-15 Sätt att ur returmaterial återvinna en eller flera polyolefiner till exempel polyeten och polypropen
SE9203027-9 1992-10-15

Publications (1)

Publication Number Publication Date
WO1994009064A1 true WO1994009064A1 (fr) 1994-04-28

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ID=20387482

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/SE1993/000836 Ceased WO1994009064A1 (fr) 1992-10-15 1993-10-13 Procede de recuperation de polythene et de polypropylene et autres polyolefines a partir de materiaux de retour, notamment ceux de type composite

Country Status (1)

Country Link
WO (1) WO1994009064A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GR1002446B (el) * 1995-12-19 1996-10-01 Μια νεα μεθοδος για την ανακυκλωση πλαστικων απορριμματων με συνδυασμο τεχνολογιας διαχωρισμου λογω διαφορετικης πυκνοτητας και τεχνολογιας διαλυσης/επανακαταβυθισης.
CN108003378A (zh) * 2017-12-08 2018-05-08 禾欣可乐丽超纤皮(嘉兴)有限公司 聚乙烯甲苯溶液中聚乙烯与甲苯的分离方法及装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2639864B2 (de) * 1975-09-02 1979-04-26 Mitsubishi Jukogyo K.K., Tokio Verfahren zur Aufarbeitung eines Gemisches aus Hochpolymerabfällen
DE2801522A1 (de) * 1978-01-13 1979-07-19 Agency Ind Science Techn Verfahren zur klassierung plastenhaltiger abfallstoffe
WO1991003515A1 (fr) * 1989-09-11 1991-03-21 Rensselaer Polytechnic Institute Recyclage de polymeres par dissolution selective

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2639864B2 (de) * 1975-09-02 1979-04-26 Mitsubishi Jukogyo K.K., Tokio Verfahren zur Aufarbeitung eines Gemisches aus Hochpolymerabfällen
DE2801522A1 (de) * 1978-01-13 1979-07-19 Agency Ind Science Techn Verfahren zur klassierung plastenhaltiger abfallstoffe
WO1991003515A1 (fr) * 1989-09-11 1991-03-21 Rensselaer Polytechnic Institute Recyclage de polymeres par dissolution selective

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GR1002446B (el) * 1995-12-19 1996-10-01 Μια νεα μεθοδος για την ανακυκλωση πλαστικων απορριμματων με συνδυασμο τεχνολογιας διαχωρισμου λογω διαφορετικης πυκνοτητας και τεχνολογιας διαλυσης/επανακαταβυθισης.
CN108003378A (zh) * 2017-12-08 2018-05-08 禾欣可乐丽超纤皮(嘉兴)有限公司 聚乙烯甲苯溶液中聚乙烯与甲苯的分离方法及装置

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