WO2018002102A1 - Procédé de fabrication d'un corps en mousse de pet - Google Patents

Procédé de fabrication d'un corps en mousse de pet Download PDF

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Publication number
WO2018002102A1
WO2018002102A1 PCT/EP2017/065929 EP2017065929W WO2018002102A1 WO 2018002102 A1 WO2018002102 A1 WO 2018002102A1 EP 2017065929 W EP2017065929 W EP 2017065929W WO 2018002102 A1 WO2018002102 A1 WO 2018002102A1
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WO
WIPO (PCT)
Prior art keywords
melt
blowing agent
bar
extruder
propellant
Prior art date
Application number
PCT/EP2017/065929
Other languages
German (de)
English (en)
Inventor
Frank Van Lück
Rolf Heusser
Original Assignee
Promix Solutions Ag, Winterthur, Ch
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 Promix Solutions Ag, Winterthur, Ch filed Critical Promix Solutions Ag, Winterthur, Ch
Publication of WO2018002102A1 publication Critical patent/WO2018002102A1/fr

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    • 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
    • B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
    • B29C44/34—Auxiliary operations
    • B29C44/36—Feeding the material to be shaped
    • B29C44/46—Feeding the material to be shaped into an open space or onto moving surfaces, i.e. to make articles of indefinite length
    • B29C44/50—Feeding the material to be shaped into an open space or onto moving surfaces, i.e. to make articles of indefinite length using pressure difference, e.g. by extrusion or by spraying
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/125—Water, e.g. hydrated salts
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/127—Mixtures of organic and inorganic blowing agents
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/141—Hydrocarbons
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/142—Compounds containing oxygen but no halogen atom
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/143—Halogen containing compounds
    • C08J9/144—Halogen containing compounds containing carbon, halogen and hydrogen only
    • C08J9/146—Halogen containing compounds containing carbon, halogen and hydrogen only only fluorine as halogen atoms
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
    • C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
    • C08J9/149—Mixtures of blowing agents covered by more than one of the groups C08J9/141 - C08J9/143
    • 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
    • B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
    • B29C44/34—Auxiliary operations
    • B29C44/3415—Heating or cooling
    • 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
    • B29K2105/04—Condition, form or state of moulded material or of the material to be shaped cellular or porous
    • B29K2105/046—Condition, form or state of moulded material or of the material to be shaped cellular or porous with closed cells
    • 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
    • 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
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/02—Foams characterised by the foaming process characterised by mechanical pre- or post-treatments
    • C08J2201/03—Extrusion of the foamable blend
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/10—Water or water-releasing compounds
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/12—Organic compounds only containing carbon, hydrogen and oxygen atoms, e.g. ketone or alcohol
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/16—Unsaturated hydrocarbons
    • C08J2203/162—Halogenated unsaturated hydrocarbons, e.g. H2C=CF2
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/18—Binary blends of expanding agents
    • C08J2203/182—Binary blends of expanding agents of physical blowing agents, e.g. acetone and butane
    • 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
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/20—Ternary blends of expanding agents
    • C08J2203/202—Ternary blends of expanding agents of physical blowing agents
    • 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

Definitions

  • plastic foams In the field of the production of plastic foams is known to produce by means of an extruder, a plastic melt, the blowing agent is added. During and after passage through a dispensing nozzle at the end of the extruder, the propellant expands to form the cells of the foam.
  • PET melts having a low IV can not achieve low densities for the foam produced, such as densities below 500 kg / m 3 .
  • a first blowing agent is added to the melt.
  • a single first propellant may be added or multiple first propellants may be added.
  • the first blowing agent may be added as a mixture of a plurality of first blowing agents or may be added as a pure substance.
  • the first blowing agent is added to the melt as a gas, liquid or solid.
  • the first blowing agent is a physical blowing agent.
  • the first blowing agent is self-adhesive, especially in PET melt.
  • the first blowing agent may be a fabric that requires a pressure of not more than 40 bar at 100 ° C to be liquid or supercritical.
  • the first blowing agent is self-nucleating. Due to the nucleating effect of the blowing agent is a variety generated by cells. It comes to cell growth, resulting in many cells with low cell volume. With an increased proportion of blowing agent, the number of cells increases.
  • the first propellant produces a high number or a high proportion of closed cells.
  • the first, self-nucleating propellant produces cells or nucleation centers in high numbers (based on the volume in which the cells are located).
  • the first propellant in addition to the function of propellant itself (i.e., volume augmentation; "driving" of cells) has the function of nucleating, i. the germination. Therefore, the process can be carried out without further blowing agents (such as particles such as talcum).
  • the prefix "self” of the term “self-nucleating” is intended to indicate this second function, i. should indicate that the first propellant itself performs the function of nucleating. Instead of "self-nucleating", the term “nucleating” can also be used.
  • Nucleating or self-nucleating propellants Propellant produces cells or nucleants in a volume concentration that is substantially equal to or greater than the volume concentration produced in foams with chemical propellant.
  • Non-nucleating propellants produce cells or nucleating centers in a volume concentration lower than the volume concentration in foams produced with chemical blowing agent.
  • the volume concentration of cells or nucleating centers in non-nucleating propellants is not more than 50%, 20% or 10% of the volume concentration in foams produced with chemical blowing agent.
  • the volume concentration of a self-nucleating propellant is above this volume concentration.
  • a second propellant is added to the melt.
  • a single second propellant may be added or several second propellants may be added.
  • the second blowing agent may be added as a mixture of a plurality of second blowing agents or may be added as a pure substance.
  • the second blowing agent is added as a gas, liquid or solid to the melt.
  • the first and second blowing agents may be added to the melt at different locations or may be added as a mixture to the melt at the same point.
  • the melt is supplied as the first and second blowing agent physical blowing agent.
  • the second propellant is preferably a physical propellant.
  • the second propellant in particular has a vapor pressure at 100 ° C, which is not more than 40 bar or at this temperature (according to a first alternative) preferably not more than 80 bar or in a second alternative at this temperature not more than 60 bar or preferably not more than 50 bar.
  • the vapor pressure depends in particular on the foam cell size to be achieved or the volume fraction of closed cells on the foam body or the desired foaming rate and can in particular be selected according to desired process parameters such as desired cooling rate and in particular depending on the first blowing agent and for example the delivery rate of the first and / or second blowing agent become.
  • the melt in addition to the first blowing agent preferably no further nucleating substance is supplied.
  • no nucleating agent is fed to the melt as a solid (or as a particle).
  • the melt passed through the dispensing nozzle preferably comprises no talc as nucleating agent, in particular no talc with particle sizes of less than 50, 20, 10 or 5 ⁇ m, in particular no talcum with particle sizes of 0.1-10 ⁇ m.
  • Cells are then destroyed under the influence (of external or internal pressures) if predetermined breaking points exist. These in turn are caused by regions of different temperature, different polymers or foreign substances in the cell wall. The foreign substances lead to notch effects or to greatly differing cell wall thickness, e.g. on average 5 microns.
  • the melt is admixed with at least one nucleating agent as a solid (in particular as a particle).
  • the second blowing agent preferably has a lower vapor pressure than the first blowing agent (in particular at 100 ° C, at 120 ° C or at 140 ° C or 160 ° C). This preferably applies to the temperature of the melt at the dispensing nozzle.
  • the first blowing agent can form nucleation centers or cells, without the second blowing agent, on passing into the gas phase, disturbing the latter or inflating it too rapidly or too strongly.
  • the second blowing agent serves in particular for the removal of heat and therefore preferably has a comparatively high (specific) heat of vaporization. By removing heat due to the phase change of the second blowing agent as the melt passes through the dispensing nozzle, the cell walls are solidified.
  • the second blowing agent preferably has a vapor pressure at 100 ° C which is equal to or less than the (vapor) pressure of the first blowing agent at 100 ° C.
  • the vapor pressure of the second blowing agent at 100 ° C. is in particular not more than 30, 35, or 40 bar, or not more than 2 or 3 bar, for example not more than 4, 6 or 8 bar, and in particular not more than 10, 15 20 or 25 bar.
  • Different steam pressures (at 100 ° C) can be used depending on the desired physical properties of the foam product to be produced or on the process parameters of the process (temperature, pressure, conveying speed, type of extruder or extruder); Due to the possible adaptations, different upper limits of 2 bar up to an upper limit of 40 bar at 100 ° C may be desirable.
  • the propellant-added plastic melt is cooled.
  • the melt can be passed through an extruder which is provided with cooling elements or which, in this way or otherwise, cools the melt.
  • the plastic melt (mixed with the blowing agent) is cooled to a desired temperature. This can be achieved by controlling the temperature of the melt to the desired temperature. In particular, this can be achieved by measuring the melt temperature, comparing with the target temperature, and adjusting the cooling according to the result of the comparison. It may be provided a control that controls the cooling, in particular the controls the cooling elements, i. their power or activation state controls.
  • the desired temperature corresponds to a foaming temperature, i. a temperature at which give desired foam properties, in particular a maximum density.
  • the foaming temperature can be, for example, within an interval of 245-270 ° C, for example in an interval of 255-265 ° C.
  • the blowing agents can be introduced into the melt at the same delivery rate (and thus in equal parts), depending on the blowing agent, plastic and desired foam product properties, the ratio of first blowing agent to second blowing agent (based on the mass rate of the feed), for example from 0.1 to 10 or from 0.5 to 2 can vary.
  • the lower limit of the ratio may be 0.05, 0.1 or 0.2 and the upper limit may be 20, 10 or 5.
  • the offset with the two blowing agents melt is passed through a dispensing nozzle or through a tool or a matrix.
  • the dispensing nozzle preferably has a slot, for example a round slot. Its width is preferably not greater than 10 mm, in particular not greater than 5 mm or 4 mm. For example, the gap width is 0.2 - 4 mm.
  • the dispensing nozzle is a nozzle suitable for producing a foam sheet or a foam body.
  • the melt mixed with both blowing agents is homogenized.
  • the melt temperature itself can be adjusted in its absolute value, depending on the desired properties of the resulting foam product. This makes sense insofar as the viscosity of the melt sets resistance to cell growth. By changing the melt temperature, the resistance to foaming can thus be adjusted in a targeted manner. The effect of resistance is very important in this process due to the use of low foaming propellants. This results in a low density of the resulting foam product as the melt strength decreases and the cells thus become larger.
  • the homogenization of the melt can be carried out by a melt cooler, for example by means of a static melt cooler, as it is offered for example by the company Promix Solutions AG, Switzerland, or is commercially available. Further, the homogenization of the melt may be carried out by a static mixer, such as a Kenics mixer.
  • a mixer may be used which has different, successive sections, such as sections which guide melt from the outside inwards to the middle of the cross section, and sections which have plates with recesses distributed over the cross section.
  • the first and the second propellant lead in the passage of the melt through the dispensing nozzle after this to an increase in volume in the cells, in particular to an increase in volume of closed cells, in particular at least 75%, 80%, preferably at least, 85% or 90% or most preferably make up at least 95% of all cells.
  • Due to the low vapor pressure compared to other propellants the cell growth rate is comparatively low, so that the cell growth is homogeneous and a large part of the cells remains closed. Thus, there is no agglomeration of cells, which would lead to an inhomogeneous cell structure of small and large cells. Together with the first, self-nucleating blowing agent, a homogeneous distribution is achieved. Furthermore, the cell walls are closed and equally thin.
  • At least one process parameter (temperature, pressure, delivery rate or the like) is adjusted in such a way that cell walls with a thickness of not more than 10 ⁇ m, 8 ⁇ m, 5 ⁇ m or 2 ⁇ m result.
  • the method is performed such that cell walls with a thickness of not more than 1 .mu.m, 0.5 .mu.m and particularly preferably not more than 0.2 .mu.m or 0.1 .mu.m result.
  • the second blowing agent removes a larger amount of heat from the melt during evaporation.
  • the specific heat of evaporation of the second blowing agent is, for example, at least 200, 300, 400, or 500, kJ / kg, preferably at least 600, 700 or kJ / kg, more preferably at least 800, 900 or 1000, especially at least 1500 or 2000 kJ / kg. Due to the thin cell walls, the removal of energy by the evaporation leads to a solidification of the melt. Due to this and the moderate increase in cell volume, the cell is stabilized and does not burst during foaming.
  • the method described here provides first to produce a PET melt.
  • the melt is produced in an extruder, in particular by supplying to the extruder polyethylene terephthalate granules (PET granules), which are melted in the extruder, or by supplying melt to the extruder, for example in an upstream unit (such as another extruder). is produced from granules.
  • PET granules polyethylene terephthalate granules
  • the PET has an intrinsic viscosity (IV) less than 0.75, resp. 0.8, in particular with a weight proportion of at least 90% (of the total plastic content of the melt).
  • the PET may be a mixture of a plurality of PET plastic materials or may be substantially made of only a PET plastic material.
  • the melt may in particular contain a proportion of PET with an IV smaller than 0.8.
  • the proportion preferably makes up at least 80% and particularly preferably at least 90%, based on the total plastic melt. The proportions are by weight.
  • a first blowing agent is added to the melt.
  • the first blowing agent is self-nucleating.
  • the first blowing agent may be added in such a way that it has a (partial) pressure of not more than 80 bar, 60 bar or 50 bar (for example 20-45 bar) in the melt. This is achieved by adding the first blowing agent at a suitable pressure and / or rate.
  • the temperature of the melt can be adjusted accordingly (since the temperature also has an effect on the pressure) or taken into account in the selection of the feed rate of the first blowing agent.
  • a first blowing agent having a critical temperature greater than 0 ° C, 60 ° C, 100 ° C, 200 ° C, or greater than 260 ° C or 280 ° C may also be used.
  • the vapor pressure at 100 ° C is not more than 40 bar, in particular not more than 35 bar and preferably not more than 32 bar.
  • the vapor pressure of the first propellant at 100 ° C may be at least 5 bar, in particular at least 10 bar and preferably at least 20 or even 25 bar or 28 bar.
  • the first propellant is supplied according to an example with a mass flow rate of the melt, which is preferably at least 0.1, 1, 2, 3%, preferably at least 4%, in particular at least 5% and particularly preferably 6% of the mass flow rate of the plastic melt.
  • the feeding of the first blowing agent can be carried out in such a way or controlled in relation to the conveying of the plastic melt that a proportion of the first blowing agent of at least 0.1 wt%, 1 wt%, or 3 wt% or 4 wt. -%, preferably at least 5 wt .-% and particularly preferably of at least 6 wt .-% based on the polymer content of the plastic melt results.
  • a first, specific embodiment provides that the first propellant has a vapor pressure at 100 ° C, which is according to a first alternative between 25 bar and 35 bar and according to a second, more specific alternative between 28 and 32 bar.
  • a second, specific embodiment provides that the first propellant has a critical temperature according to a first alternative between 100 ° C and 120 ° C and according to a second, more specific alternative, a critical temperature between 105 ° C and 115 ° C.
  • a third, specific embodiment provides that the first propellant has a critical pressure according to a first alternative between 30 bar and 42 bar according to a second, more specific alternative, a critical pressure between 38 bar and 40 bar.
  • An alternative possibility would be that nitrogen is used as the first blowing agent.
  • a second blowing agent is added to the melt.
  • the second blowing agent preferably has a low vapor pressure at 100 ° C compared to the first blowing agent, in particular less than 90%, 75%, preferably less than 3/4 or 2/3 and especially less than 1/3 or particularly preferably less may be 1/5 or 1/10 of the vapor pressure of the first propellant at 100 ° C.
  • the vapor pressure of the second blowing agent at 100 ° C is not more than 7 bar, in particular not more than 5 bar and preferably not more than 3 bar or 2.5 bar.
  • the vapor pressure of the second blowing agent at 100 ° C. can be at least 1.5 bar, in particular at least 1.7 bar and preferably at least 2 or even at least 2.1 bar.
  • the temperature of the melt as it passes through the outlet nozzle is for example 240 ° C - 300 ° C, preferably 250 - 270 ° C.
  • a first, specific embodiment provides that the second propellant has a vapor pressure at 100 ° C, which is according to a first alternative between 2 bar and 4 bar and according to a second, more specific alternative between 2 and 3 bar.
  • a second, specific embodiment provides that the second propellant has a critical temperature according to a first alternative between 200 ° C and 280 ° C and according to a second, more specific alternative, a critical temperature between 230 ° C and 260 ° C.
  • a third, specific embodiment provides that the second propellant has a critical pressure according to a first alternative between 50 bar and 80 bar according to a second, more specific alternative has a critical pressure between 58 bar and 68 bar.
  • the critical temperature of the second propellant is not more than 100 ° C, more preferably not more than 90 ° C and preferably not more than 80 ° C above the temperature of the plastic melt as it passes through the dispensing nozzle.
  • the melt to which the first and second blowing agents have been added is homogenized, in particular to achieve a homogeneous distribution of the blowing agents in the melt.
  • the first blowing agent may have a molecular weight of at least 20.70 g / mol, preferably of at least 90 g / mol and preferably of at least 100 g / mol.
  • the molecular weight is at least 110 g / mol, preferably at least 112 g / mol and more preferably at least 114 g / mol.
  • the second propellant has a specific heat of vaporization of at least 200, 300, 400, preferably at least 500 or 600, more preferably 700 or 750 kJ / kg, and according to a specific embodiment preferably at least 780 kJ / kg or for example at least 820 kJ / kg.
  • the heat of vaporization is removed during the phase change (evaporation) of the plastic melt, in particular the cell walls.
  • the associated cooling takes place after the (self-nucleating) first blowing agent has already formed cells in the melt or after cell growth has already begun.
  • the cooling of the cell walls caused by the phase transformation of the second propellant takes place after the cells have already reached a part of their final volume.
  • Increasing the resistance of the cell wall prevents the cells from over-inflating. Since no PET with an IV> 0.8 is used in this procedure, the cells would otherwise burst and cell agglomeration would occur.
  • the first and / or the second blowing agent may be organic compounds.
  • the first propellant is, for example, a hydrofluoroolefin.
  • a first propellant preferably 1,3,3,3-tetrafluoropropene (trans-1,3,3,3-tetrafluoroprop-1-ene) is used, which also as R-1234ze (E) (according to the ASHRAE Standard 34) referred to and sold under the trade name R-134.
  • This first propellant has a vapor pressure of about 30 bar (29.9 bar) at 100 ° C, a critical temperature of about 109 ° C (109.4 ° C) and a critical pressure of about 36 bar (36.36 bar) on.
  • this first blowing agent has a molar mass of about 114 g / mol (114.04 g / mol) and a specific heat capacity of about 1 kJ / kg ° K (0.9822 kJ / kg ° K).
  • nitrogen may be the first blowing agent.
  • the first propellant can thus be present in the supercritical state in the melt or be supplied in the supercritical state of the melt.
  • the second propellant may be an alcohol, an alkane, an ester or water or a mixture of at least two of these substances.
  • the second propellant is preferably an alcohol, especially with less than 4 carbon atoms (to ensure a minimum evaporation pressure), but it may also be an alkane or an alkene.
  • the second blowing agent may be an alkane or alkene having more than 5, 6 or 7 carbon atoms (in particular to ensure maximum evaporation enthalpy).
  • the second blowing agent may be octane (boiling point 126 ° C, molar mass 114 g / mol) or heptane (boiling point 98 ° C, molar mass 100 g / mol).
  • the second propellant may have a vapor pressure of about 0.5 bar at 100 ° C (or about 2.4 bar at 160 ° C), such as is true for octane.
  • the second blowing agent may have a vapor pressure of about 1 bar at 100 ° C (or about 4.6 bar at 160 ° C), as is true for heptane.
  • the second propellant may have a vapor pressure of about 2.4 bar at 100 ° C (or about 9 bar at 160 ° C), as is true for hexane.
  • the second blowing agent may have a vapor pressure of about 7.5 bar at 100 ° C, as is true for pentane.
  • the vapor pressure of the second blowing agent at 100 ° C. can, for example, be 0.4 to 0.6 bar, 0.9 to 1.1 bar, 2 to 3 bar or 7 to 8 bar, in accordance with specific embodiments of the procedure described here. It is also possible intermediate values such as 0.6- 0.9 bar or 1.1-2 bar or 3-7 bar (at 100 ° C), or pressures of less than 0.4 bar or more than 10 bar, depending on the blowing agent used.
  • the second blowing agent may have a molar mass of at least 55, 70, 80, 100 or 110 g / mol.
  • the second propellant may have a molar mass of at least 55 g / mol at a boiling pressure of not more than 19 bar at 100 ° C., as is the case for butane, for example.
  • the second propellant may have a molar mass of at least 70 g / mol at a boiling pressure of not more than 7.5 bar at 100 ° C., as is the case, for example, with pentane.
  • the second propellant may have a molar mass of at least 85 g / mol at a boiling pressure of not more than 3 bar at 100 ° C., as is the case, for example, with hexane.
  • the second blowing agent can have a molar mass of at least 100 g / mol at a boiling pressure of not more than 1.2 bar at 100 ° C., as is the case for example with heptane.
  • the second propellant may have a molar mass of at least 110 g / mol at a boiling pressure of not more than 0.4 bar at 100 ° C. (or not more than 3 bar at 160 ° C.), such as for octane is the case.
  • ethanol is considered as a second blowing agent in particular.
  • the second blowing agent may therefore have a vapor pressure at 100 ° C, which is in the range of 2 - 2.5 bar (ethanol: 2.25 bar).
  • ethanol has a critical temperature of about 240 ° C. (243.1 ° C.) and a critical pressure of about 60-65 bar (63.8 bar).
  • the second blowing agent may have a molar mass between 30 g / mol and 60 g / mol, in particular of about 45 g / mol (46 g / mol).
  • the specific heat of vaporization of this second blowing agent is between 800 and 900 kJ / kg, in particular about 845 kJ / kg.
  • the specific heat capacity of this second propellant is about 2.4 kJ / kg ° K (2.43 kJ / kg ° K).
  • propanol considered as a second blowing agent.
  • the second propellant may therefore have a vapor pressure at 100 ° C, which is in the range of 1.75 - 2.25 bar (ethanol: 2 bar).
  • the second propellant may have a molar mass between 40 g / mol and 80 g / mol, in particular of about 88 g / mol (approximately in the case of propanol).
  • the specific heat of vaporization of this second blowing agent is between 500 and 800 kJ / kg, in particular between 600 and 700 kJ / kg, in particular about 665 kJ / kg. Hexanol can also be considered as the second blowing agent.
  • an ether is considered as a second blowing agent.
  • ethers with a boiling point below 100 ° C or below 70 ° C can be used, in particular with a boiling point of below 40 ° C and specifically below 0 ° C.
  • an open-chain ether such as dimethyl ether or diethyl ether may be used, or a cyclic ether such as tetrahydrofuran may be used.
  • water is considered as blowing agent, in particular due to the high heat of vaporization of more than 2000 kJ / kg.
  • the second blowing agents mentioned herein may be used singly or as a mixture of two or more than two of the blowing agents mentioned herein.
  • the second blowing agents referred to herein can be used as a mixture of two or more polar blowing agents or of two or more nonpolar blowing agents.
  • a third propellant may be used, or several other propellants (in addition to the first and second propellants) may be used.
  • the method may include the step of homogenizing the melt.
  • This refers in particular to the melt mixed with the first and the second blowing agent.
  • the melt is homogenized according to a maximum temperature difference at the dispensing nozzle of not more than + - 2, preferably not more than + -1, more preferably not more than + -0.5 ° C.
  • Static mixing elements are used here. These are arranged with the proviso and designed to unify the melt temperature over the cross-section of the melt (in particular immediately before the dispensing nozzle). This concerns in particular the design, for example the size and the length and / or the number.
  • web mixing parts are used here, since the melt temperature can be more uniformly standardized on account of the transverse flow component.
  • the melt is tempered.
  • the melt is preferably cooled to a desired temperature for foaming.
  • the target temperature is preferably not more than 50 ° C or not more than 30 ° C below the melting temperature of the original plastic melt during melting.
  • the melt can already be tempered or cooled during homogenization.
  • the melt is cooled before being passed through the dispensing nozzle.
  • the process is set such that after the mixer all machine components are set to the desired melt temperature (dispensing nozzle, adapter flanges, etc.).
  • the method can therefore be carried out with an extruder device that has tempering elements, in particular heating elements and / or cooling elements.
  • the melt is preferably tempered, in particular cooled.
  • An extruder apparatus having a melt homogenizer which is itself cooled may be used.
  • the extruder device used has a dispensing nozzle which follows the melt homogenizer and which is cooled.
  • the dispensing nozzle, through which the melt is passed, can be followed by a flange connection directly onto the melt homogenizer, in which the melt is homogenized.
  • the melt is cooled immediately after homogenization (and optionally also during homogenization).
  • the homogenizing step is followed directly by the step of passing the melt through the dispensing nozzle.
  • the melt is preferably passed through a cooled dispensing nozzle.
  • the dispensing nozzle and possibly a connecting element which connects the melt homogenizer with the dispensing nozzle (such as a flange) are heated to a desired temperature, in particular by cooling.
  • the dispensing nozzle and possibly the connecting element can have a tempering element, in particular a cooling element.
  • the temperature control element may have a heat fluid channel which is connected to a heat source or a heat exchanger. It may be provided a control unit, which performs the step of tempering according to a target temperature as the control target.
  • an extruder which conveys the plastic melt and by means of which the first blowing agent, the second blowing agent or both blowing agents are introduced into the plastic melt.
  • Another extruder can be used in which the melt (from granules) is produced.
  • the melt or the plastic granules can be heated to melt. The heating preferably takes place before homogenization. The heating may be performed in accordance with a target heat output or may be performed in the sense of control with a target temperature as the control target. After homogenization and / or while passing the melt through the dispensing nozzle, the melt is preferably cooled or cooled according to a desired temperature (in the sense of a control target).
  • the extruder in which the plastic melt is produced or plastic granules are heated, promotes the melt in the extruder, which has the dispensing nozzle. Furthermore, three sequential extruders can be used: a first extruder for melting the granules, i. for producing the melt, a second extruder (following the first extruder) within which at least one of the blowing agents or additives (such as paint or flame retardant) are fed to the melt and blended, and a third extruder (following the second extruder), which cools the mixture and has the discharge nozzle at the end.
  • a first extruder for melting the granules i. for producing the melt
  • a second extruder within which at least one of the blowing agents or additives (such as paint or flame retardant) are fed to the melt and blended
  • a third extruder following the second extruder
  • FIG. 1 shows an extrusion system which can be used to carry out the method.
  • the individual components are not drawn to scale or according to a real aspect ratio.
  • the size ratios of the components do not reflect their real size. Rather, the representation serves only the overview and the explanation of the functional links between the elements.
  • a granulate feed GZ is fed to a melting extruder AE (i.e., a first extruder) as a solid PET plastic.
  • the melting extruder AE has a first drive A1, which drives the extruder screw of the melting extruder AE.
  • the melting extruder has at least one heating element H1-H3.
  • the heating elements are exemplified as three heating elements H1 - H3. These are arranged one after the other.
  • the heat of the heating elements leads to the melting of the plastic melt in the melting extruder AE and heat the plastic melt to a temperature of about 200 ° C - 320 ° C, for example to 270 ° C.
  • the heating elements may be electrical heating elements, or have coloursfluidkanäle which are connected to a heat source.
  • the blowing agents T1, T2, i. the first blowing agent T1 and the second blowing agent T2 are introduced into the melt in the melt-down extruder AE in the illustrated example, but can also be introduced into the melt in the cooling extruder KE.
  • the blowing agents T1, T2 can be introduced into the melt in different extruders or in equal extruders, especially if only one extruder is used, i. an extruder in which the melt is produced and through the discharge nozzle of the melt is guided (and possibly also homogenized).
  • the first extruder i.e., the melting extruder AE
  • the at least one first blowing agent T1 and the at least one second blowing agent T2 are added to the melt.
  • the illustrated example provides that in a first extruder (the melting extruder AE), the melt is produced and at the end of a second extruder (the cooling extruder KE) the melt is passed through a dispensing nozzle D, in particular after prior homogenization by a melt homogenizer M.
  • the end of the reflow extruder AE opposite the feed of granules is connected via an intermediate piece Z to a cooling extruder KE.
  • the cooling extruder KE as the second extruder, follows the melting extruder AE as the first extruder.
  • the intermediate piece Z may be formed as a connecting line.
  • the cooling extruder KE has a drive A2.
  • the cooling extruder KE has at least one cooling element K1, K2.
  • the cooling elements K1, K2 are exemplified.
  • the cooling elements K1 and K2 act on the extruder body itself.
  • the cooling element K3 acts on a dispensing nozzle D.
  • the dispensing nozzle D adjoins a melt homogenizer or mixer M.
  • the melt homogenizer M has a cooling element K3 ', which acts on the melt in the homogenizer M.
  • the melt homogenizer M connects the cooling extruder KE with the dispensing nozzle D.
  • the melt homogenizer M thus follows the cooling extruder KE.
  • the melt homogenizer M and the subsequent dispensing nozzle D connect to that end of the cooling extruder KE, which is opposite to the intermediate piece.
  • the cooling elements K1 and K2 are arranged one after the other. This also applies to the cooling elements K3 'and K3.
  • the cooling elements K3 and K3 ' cool the melt to suitable temperature for foaming. This is in particular less than 280 ° C, for example to 270 ° C at the dispensing nozzle D.
  • the dispensing nozzle D can be designed as a round-slot nozzle, or as a slot die.
  • the dispensing nozzle D emits a plastic web (closed in cross-section).
  • the dispensing nozzle D is designed as a foam tool.
  • the melt homogenizer M is connected upstream of the dispensing nozzle D.
  • the mixer M connects the cooling extruder KE with the dispensing nozzle D.
  • the mixer is in particular a static mixer, for example a mixer of the Sulzer® SMX type.
  • the filter F may be part of the intermediate piece Z.
  • a control or regulation can be provided which acts on the drives A1 and A2 and which acts on heating elements H1-H3 and on the cooling elements K1, K2.
  • partial control units SR1-4 are shown.
  • the sub-control unit SR1 controls the cooling elements K1, K2, K3 and K3 '(or a heat exchanger or another cold source connected thereto).
  • the sub-control unit SR1 regulates in particular the cooling elements K3, K3 'to a desired temperature, which is suitable in particular for foaming.
  • the sub-control unit SR2 controls the drive A2 of the cooling extruder KE.
  • the sub-control unit SR3 controls the drive A1 of the Aufschmelzextruders AE.
  • the sub-control unit SR4 controls the heating elements H1-H3 of the reflow extruder AE.
  • the arrows emanating from the sub-control units represent the activation of the relevant elements symbolically.
  • the control is set to a desired temperature (at the dispensing nozzle D), which regulates said elements according to this temperature.
  • the combination of the control with the mixer M allows a thermal homogenization of the melt and in particular the adjustment of the foam S to a specific density.
  • quantities such as the proportion of blowing agent and the desired or actual material distribution between the cell wall and cell interspace act on the properties of the foam, so that these variables are also taken into account (at least indirectly) in the control or regulation of the temperature.
  • the foam body results in the cooling and thus hardening of the foam S after exiting the respective extruder.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un corps en mousse de PET. Du PET fondu est élaboré dans une extrudeuse (AE). Un ou plusieurs premiers agents gonflants (T1) autonucléants sont ajoutés. Un deuxième agent gonflant (T2) est ajouté, lequel présente une pression de vapeur ne dépassant pas 40 bars à 100°C. Le PET fondu mélangé avec le premier et le deuxième agent gonflant (T1 ; T2) est homogénéisé. S'en suivent les étapes de refroidissement du mélange à une température de consigne et (f) d'acheminement du PET fondu homogénéisé à travers une buse de sortie.
PCT/EP2017/065929 2016-07-01 2017-06-27 Procédé de fabrication d'un corps en mousse de pet WO2018002102A1 (fr)

Applications Claiming Priority (2)

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DE102016008038.8 2016-07-01
DE102016008038.8A DE102016008038B4 (de) 2016-07-01 2016-07-01 Verfahren zur Herstellung eines PET-Schaumkörpers

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WO2023019920A1 (fr) * 2021-08-16 2023-02-23 江苏大毛牛新材料有限公司 Procédé de préparation de matériau cellulaire par moussage d'azote

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5679295A (en) * 1996-07-11 1997-10-21 Genpak Corporation Method for producing polyester foam using a blowing agent combination
US20040241418A1 (en) * 2001-03-16 2004-12-02 Cahill Paul J. Composites for railroad ties and other products
EP2277969A2 (fr) * 2004-04-29 2011-01-26 Honeywell International Inc. Compositions contenant des oléfines substituées par du fluor
US20120232175A1 (en) * 2011-03-11 2012-09-13 Mucell Extrusion, Llc Pet foam articles and related methods
EP2504385A1 (fr) * 2009-11-24 2012-10-03 Aixfotec GmbH Procédé de fabrication de granulés de pet et granulés de pet

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3930847A1 (de) 1989-09-15 1991-04-04 Berstorff Gmbh Masch Hermann Verfahren zum herstellen eines schaumstoffes aus thermoplastischem kunststoff und extruderanlage zur durchfuehrung des verfahrens

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5679295A (en) * 1996-07-11 1997-10-21 Genpak Corporation Method for producing polyester foam using a blowing agent combination
US20040241418A1 (en) * 2001-03-16 2004-12-02 Cahill Paul J. Composites for railroad ties and other products
EP2277969A2 (fr) * 2004-04-29 2011-01-26 Honeywell International Inc. Compositions contenant des oléfines substituées par du fluor
EP2504385A1 (fr) * 2009-11-24 2012-10-03 Aixfotec GmbH Procédé de fabrication de granulés de pet et granulés de pet
US20120232175A1 (en) * 2011-03-11 2012-09-13 Mucell Extrusion, Llc Pet foam articles and related methods

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