EP4308355A1 - Procédé de production de particules d'élastomère thermoplastique expansé - Google Patents

Procédé de production de particules d'élastomère thermoplastique expansé

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Publication number
EP4308355A1
EP4308355A1 EP22711984.9A EP22711984A EP4308355A1 EP 4308355 A1 EP4308355 A1 EP 4308355A1 EP 22711984 A EP22711984 A EP 22711984A EP 4308355 A1 EP4308355 A1 EP 4308355A1
Authority
EP
European Patent Office
Prior art keywords
wax
liquid
foam particles
thermoplastic elastomer
blowing agent
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.)
Withdrawn
Application number
EP22711984.9A
Other languages
German (de)
English (en)
Inventor
Lisa Marie Schmidt
Matthias GOLDBECK
Uwe Keppeler
Franziska DENNHARDT
Theresa HUELSMANN
Florian Tobias RAPP
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Publication of EP4308355A1 publication Critical patent/EP4308355A1/fr
Withdrawn legal-status Critical Current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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/16—Making expandable particles
    • 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
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B29B9/065—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion under-water, e.g. underwater pelletizers
    • 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
    • B29B9/00—Making granules
    • B29B9/12—Making granules characterised by structure or composition
    • 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
    • B29B9/00—Making granules
    • B29B9/16—Auxiliary treatment of granules
    • 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
    • C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
    • 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
    • C08J9/16—Making expandable particles
    • C08J9/18—Making expandable particles by impregnating polymer particles with the blowing agent
    • 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
    • C08J9/22—After-treatment of expandable particles; Forming foamed products
    • C08J9/224—Surface treatment
    • 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
    • B29B9/00—Making granules
    • B29B9/16—Auxiliary treatment of granules
    • B29B2009/163—Coating, i.e. applying a layer of liquid or solid material on the granule
    • 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
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • 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
    • B29K2021/00—Use of unspecified rubbers as moulding material
    • B29K2021/003—Thermoplastic elastomers
    • 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
    • B29K2075/00—Use of PU, i.e. polyureas or polyurethanes 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
    • 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
    • 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
    • C08J2203/06—CO2, N2 or noble gases
    • 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
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • 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
    • C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
    • C08J2375/04—Polyurethanes
    • C08J2375/08—Polyurethanes from polyethers

Definitions

  • the invention relates to foam particles made from an expanded thermoplastic elastomer and a method for producing such particles.
  • Foam particles made of expanded thermoplastic elastomer can be used in many areas, for example in the production of molded parts such as packaging materials, seat cushions, car seats, mattresses, floor coverings, tires, saddles or soles of running shoes.
  • the foam particles are placed in a tool, for example, and are subjected to steam or heated there, so that they fuse with one another on the outside.
  • the production of the moldings from the foam particles usually takes place at different locations than the production of the foam particles, it is necessary to transport them from the location of the manufacture of the foam particles to the location of the molding production.
  • the transport usually takes place in large containers, for example big bags or octabins. These are filled and emptied via conveyors, with the material of the foam particles and the geometry and bulk density of the foam particles having a major impact on transport behavior. Even if the production of the foam particles and the production of the molded parts take place in neighboring plants, it is necessary to first store the material before it can be further processed.
  • the foam particles are stored in a large container or in a stationary storage container, they can agglomerate to a great extent, so that removal from the large container or storage container using conveying devices (e.g. pneumatic suction lances) known to those skilled in the art is not possible without additional mechanical loosening .
  • conveying devices e.g. pneumatic suction lances
  • thermoplastic polyurethane Processes for producing foam particles from a thermoplastic polyurethane are described, for example, in WO-A 2007/082838.
  • a granulate is first produced from the thermoplastic polyurethane and this is then placed in a suspension under pressure and at a temperature above the softening point of the poly mers impregnated with a blowing agent and expanded to foam particles by relaxation.
  • the blowing agent can also be added in an extruder and the foam particles are produced by expansion in an underwater granulation.
  • the water usually contains a granulation aid that remains on the foam particles. However, this is not sufficient to prevent blocking in the storage container or large container.
  • a further disadvantage of the methods known from the prior art is that even a small amount of lubricant that is added during production can have the effect that the welding of the foam particles to form the desired molded part is impeded.
  • the object of the present invention was therefore to provide a process for the production of foam material particles which can be processed further during storage without the risk of blocking.
  • the task is solved by a process for the production of foam particles, comprising:
  • thermoplastic elastomer melt (a) mixing a thermoplastic elastomer melt with a blowing agent in an extruder;
  • thermoplastic elastomer melt mixed with the blowing agent through a perforated plate into a pelletizing chamber
  • the liquid in the granulation chamber contains wax, which accumulates on the surface of the granules during cutting and expanding in the granulation chamber,
  • the process produces foam particles from an expanded thermoplastic elastomer, which have a surface on which a wax is applied, the proportion of wax being 0.001 to 0.5% by weight.
  • the wax acts as a lubricant that prevents the foam particles from sticking together, so that they can be removed from the containers used for storage and transport, such as cardboard drums, silos, big bags or octabins, and conveyed without blocking.
  • a further advantage of using a wax as a lubricant is that it does not impede the subsequent processing of the foam particles and, in the concentration range described above, has in particular no negative influence on the welding of the particles to form the molded part.
  • the liquid in the granulating chamber contains the wax that accumulates on the foam particles during cutting and expanding in the granulating chamber, or the wax is applied after separating from the liquid and drying the foam particles
  • the wax is particularly advantageous to apply the wax to the surface of the foam particles or granules in the apparatus, in which the granules expand to form the foam particles as a result of relaxation of the propellant, since each time transport is carried out without a lubricant, we already have kende wax on the surface blocking can occur. It is therefore particularly preferred if the liquid in the granulation chamber contains the wax that accumulates on the surface of the granulate during cutting and expansion in the granulation chamber.
  • the foam particles are produced by extrusion processes known to those skilled in the art, as described, for example, in WO-A 2007/082838 or WO-A 94/20568.
  • thermoplastic elastomer granules of the thermoplastic elastomer are added to the extruder, as described, for example, in WO-A 2013/153190.
  • extruder it is also possible to use the extruder to produce the thermoplastic Elastomers required starting materials, in particular the monomers from which the thermoplastic elastomer is built, and optionally add additives such as catalysts, plasticizers, stabilizers or dyes and then foam the material, as described for example in WO-A 2015/055811.
  • thermoplastic elastomer melt When the extruder is fed with the starting materials required for producing the thermoplastic elastomer, these are converted into the thermoplastic elastomer after they have been fed into the extruder, with the thermoplastic elastomer melt being produced.
  • the production takes place under the conditions known to those skilled in the art for the production of a thermoplastic elastomer in an extruder.
  • the blowing agent can then be added via a suitable addition point in step (a) and mixed with the thermoplastic elastomer melt in the extruder.
  • thermoplastic elastomer is not produced in an extruder but in any other reactor, it is also possible to introduce the thermoplastic elastomer melt produced in this way into an extruder and to mix it with the blowing agent there.
  • thermoplastic elastomer in a manner known to those skilled in the art and to feed these to the extruder in which the blowing agent is added.
  • the granules are first compressed in the feed zone of the extruder and heated in the process so that they begin to melt. The granules are then completely melted. After melting, the blowing agent can then be added, which is mixed into the thermoplastic elastomer melt using a suitable screw geometry.
  • the rotation of the screw in the extruder homogeneously mixes the thermoplastic elastomer melt with the blowing agent and transports it to the downstream unit that closes the extruder.
  • This subsequent unit can already be the perforated plate or an apparatus upstream of the perforated plate, such as a melt pump, a diverter valve, a static mixer or a melt filter or a combination of these.
  • Suitable blowing agents are, for example, halogenated hydrocarbons, saturated aliphatic hydrocarbons or inorganic gases, for example saturated hydrocarbons having 3 to 8 carbon atoms, nitrogen, air, ammonia, carbon dioxide or mixtures thereof.
  • thermoplastic elastomer melt mixed with the blowing agent is then pressed in step (b) through the perforated plate into a pelletizing chamber.
  • a knife runs on the perforated plate in the granulation chamber, with which the exiting thermoplastic elastomer melt mixed with the blowing agent is cut into granules.
  • a liquid flows through the pelletizing chamber so that the thermoplastic elastomer melt is pressed through the perforated plate directly into the liquid.
  • the pressure of the liquid flowing through the granulation chamber is selected in such a way that the thermoplastic elastomer melt emerging through the perforated plate expands until a desired density is achieved for the resulting foam.
  • the pressure of the liquid flowing through the granulation chamber is preferably in the range from 1 to 20 bar, more preferably in the range from 5 to 15 bar and in particular in the range from 7 to 12 bar.
  • the temperature of the liquid is selected in such a way that the emerging thermoplastic elastomer melt solidifies in the liquid to form the foam particles, with the melt only being allowed to solidify after the desired expansion.
  • the temperature here depends on the thermoplastic elastomer used and is preferably from 25 to 90.degree. C., more preferably from 30 to 60.degree. C. and in particular from 35 to 50.degree
  • the foam particles produced in this way are discharged from the granulation chamber with the liquid flowing through the granulation chamber and are separated from the liquid in a suitable device for solid/liquid separation. After separating from the liquid, the foam particles can be dried. The drying can take place in any suitable dryer known to those skilled in the art, for example a heated fluidized bed or silo drying.
  • the temperature of the perforated plate is preferably in a range from 20 to 110° C. above the melting point of the thermoplastic elastomer, more preferably in a range from 50 to 90° C. above the melting point of the thermoplastic elastomer and in particular in a range from 60 to 80 °C above the melting temperature of the thermoplastic elastomer.
  • the melting temperature is the temperature that corresponds to the highest peak in differential scanning calorimetry (DSC).
  • the liquid that flows through the granulation chamber is preferably water and optionally contains a granulation aid.
  • the granulation aid serves in particular to ensure that the foam particles do not agglomerate in the liquid but remain in the liquid as individual grains.
  • Surfactants, waxes or white oils, in particular waxes or white oils, are suitable as granulation aids, for example.
  • the wax in which the wax is dispersed in the liquid flowing through the granulation chamber, the wax is applied to the granulate during expansion and solidification to form the foam particles.
  • a uniform distribution of the wax on the surface of the foam particles results in particular from the fact that with good mixing of the liquid the lubricant is present in the liquid and is evenly distributed the particles are mixed in the liquid during the expansion and solidification and the subsequent transport from the granulation chamber. The mixing results in particular from the flow of the liquid through the granulation chamber.
  • the wax Due to the movement of the foam particles in the liquid, the wax accumulates on the surface of the foam particles and at most penetrates a small part into the foam particles. This has the advantage over using wax as an additive in the setting of the polymer that in a component made from the foam particles wax can only diffuse to the surface to a very small extent if the expanded during the setting Foam particles wax has diffused into the foam particles.
  • the wax can be contained as a solid in the liquid in a dispersion or as a liquid in the liquid in an emulsion. If the wax is dispersed as a solid in the liquid flowing through the granulation chamber, it is particularly preferred if the wax is present as a powder with a particle diameter D50 in the range from 10 to 50 ⁇ m. It may be necessary to add a suspension aid to keep the wax in dispersion.
  • particle diameter with non-spherical particles is understood as meaning the geometric equivalent diameter which corresponds to the sphere diameter of a sphere of the same volume.
  • the wax acting as a lubricant can also be applied after the foam particles have been separated from the liquid and optionally dried.
  • the granules either in the form of a suspension or solution or alternatively in solid form, in which case the wax is present as a fine powder.
  • the application after the expansion of the granules can either be an alternative or in addition to the application during the expansion and solidification in the granulation chamber. follow. Additional application is required when the amount of lubricant applied to the foam particles in the pelletizing chamber during expansion and solidification is insufficient.
  • the composition of the liquid with the wax particularly preferably corresponds to the above-described composition of the liquid in which the foam particles are impregnated in the granulation chamber in the first variant (i).
  • the wax is applied to the foam particles in the form of a powder.
  • the wax and the foam particles are introduced into a container which is then closed and subsequently moved so that the foam particles collide against one another and against the wall of the container.
  • the powdery wax and the foam particles are intensively mixed with one another and the wax settles on the surface of the foam particles. The greater the force with which the foam particles collide against each other or against the wall, the better the wax adheres to the foam particles.
  • the ratio of granules to wax is in the range from 0.001 to 0.5% by weight based on the total mass of the foam particles, more preferably in the range from 0.005 to 0 .25% by weight and in particular 0.01 to 0.1% by weight. This amount is sufficient to deposit enough wax on the surface of the foam particles.
  • the individual grains of the wax in powder form preferably have a particle diameter D50 in the range from 10 to 50 ⁇ m.
  • the wax is preferably applied to the foam particles in variant (ii) at ambient pressure and ambient temperature. However, it is also possible to apply the wax to the foam particles at elevated pressure or elevated temperature. To prevent foam particles from agglomerating, the wax is applied at a temperature below the softening point. However, it is particularly preferred to apply the wax at ambient temperature.
  • the lubricating wax is ethylenebisstearylamide.
  • ethylenebisstearylamide as a lubricant has the advantage that it does not impede the processing of the foam particles and therefore does not have to be washed off in an additional process step.
  • thermoplastic elastomer As a thermoplastic elastomer is suitable in the context of the present invention, any ther moplastic elastomer that can be expanded to form foam particles and in which a Granules impregnated with a propellant by the method described above who can. Suitable thermoplastic elastomers are known per se to those skilled in the art. Suitable thermoplastic elastomers are described, for example, in “Flandbook of Thermoplastic Elastomers", 2nd edition June 2014.
  • the thermoplastic elastomer can be a thermoplastic polyurethane, a thermoplastic polyetheramide, a polyetherester, a polyesterester, an olefin-based thermoplastic elastomer, a crosslinked olefin-based thermoplastic elastomer or a thermoplastic vulcanizate, or a thermoplastic styrene-butadiene block copolymer.
  • the thermoplastic elastomer is a thermoplastic polyurethane, a thermoplastic polyetheramide, a polyetherester, or a polyesterester.
  • the thermoplastic elastomer is particularly preferably a thermoplastic polyurethane.
  • thermoplastic polyurethanes TPU
  • MFR melt flow rate
  • e-TPU expanded thermoplastic polyurethane
  • a batch mixer was switched on after drying in a bulk material heat exchanger (BFFIE, bulk flow heat exchanger).
  • BFFIE bulk material heat exchanger
  • Application by means of a suspension takes place in two different ways (experiment II and III).
  • test II the plastic particles were removed after the BFFIE and coated in a laboratory mixer.
  • trial III the lubricant was added in the granulation chamber.
  • composition of the TPU and the melt flow rate of the different TPUs are listed in Table 1.
  • the e-TPU is produced on a twin-screw extruder (Berstorff ZE 40) with a screw of 44 mm and an L/D ratio of 48, followed by a melt pump, a diverter valve with a screen changer, a perforated plate and a pelletizing chamber for underwater pelletizing .
  • the TPU was predried for 3 hours at 80° C. to a residual moisture content of less than 0.02% by weight.
  • modified TPU 1% by weight of another thermoplastic polyurethane is metered in (modified TPU).
  • modified TPU is a TPU that was compounded with 4,4'-diphenylmethane diisocyanate with an average functionality of 2.05 in a separate extrusion process.
  • the materials are melted and mixed in the extruder.
  • a mixture of CO2 and N2 is then added as a blowing agent.
  • the polymer is homogeneously mixed in the remaining extruder zones. This mixture is pressed by a melt pump via the diverter valve and the screen changer and finally through a perforated plate into the pelletizing chamber. There the mixture is cut into granules and foamed in a pressurized, temperature-controlled water system. The flow of water transports the pearls created in this way to a centrifugal dryer, where they are separated from the water flow.
  • the total throughput of the extruder was adjusted to 40 kg/h (including polymers, blowing agents).
  • composition of the blowing agent is listed in Table 3.
  • Table 3 Propellant composition used and lubricant metered into the granulation chamber
  • Experiment I Application of the lubricant as a powder
  • the lubricant was metered into the granulation chamber for the underwater granulation during the foaming process in the extruder.
  • the concentration used is listed in Table 3.
  • the blocking tendency of the particles was evaluated for all materials, with the exception of reference 3 and example 6, using a simple caking test according to method 1.
  • the evaluation was carried out by filling the fresh material into 200 L metal drums, which are lined on the inside with an inliner made of polyethylene film.
  • the barrel was filled with the material produced and immediately after filling was tempered in a circulating air oven at 60 °C for 2 h and then stored for 12 days at ambient conditions ( ⁇ 25 °C). After 12 days, the barrels were rotated 150′′ with the help of a jack so the opening was facing down. If the material trickled out of the metal barrel through the sloping surface by gravity alone, it is considered not to have blocked. If the material remains in the metal barrel despite being rotated, it is considered blocked.
  • the experimental setup consists of two components, a steel cylinder (consisting of 2 half-shells that are held together with a hose clamp and a tripod to which a movable stamp with a mass of around 1 kg is attached.
  • the cylinder has a diameter of 11 mm, the des The stamp is slightly smaller so that it can slide into the cylinder without touching it when it is in the middle below.
  • the cylinder is completely filled with e-TPU for the test.
  • the stamp is then placed on the E-TPU without applying any pressure Care must be taken to ensure that the stamp does not rest anywhere on the cylinder.
  • the weight exerted on the e-TPU is intended to simulate the pressure that would act on the material inside an octabin or big bag.
  • the tensile strength is determined for a panel thickness of 10 mm (thickness may vary slightly depending on shrinkage) based on ASTM D5035, 2015, which was drawn up for textiles. The determination is carried out using a testing machine with a 1 or 2.5 kN force transducer (class 0.5 (from 10N) according to DIN EN ISO 7500-1, 2018), long-travel transducer, traverse (class 1 or better according to DIN EN ISO 9513 , 2013) and pneumatic clamps (6 bar (with clamping jaw inserts made of pyramid grid (Zwick T600 R)).
  • the required test specimens are 150 mm x 25.4 mm in size from a 200 x 200 x 10 mm test plate (dimensions can vary slightly depending on the shrinkage).
  • test panels used were conditioned beforehand for at least 16 hours in a standard climate (23 ⁇ 2 °C and 50 ⁇ 5% air humidity).
  • the tensile test is also carried out in this standard climate the mass (precision balance; readability: ⁇ 0.001 g) of the test specimen and its thickness (probe; readability: ⁇ 0.01 mm, contact pressure 100 Pa, value is determined only once in the middle of the test specimen) are determined. From the mass, the measured thickness and the fixed values for L length (150 mm) and width (25.4 mm), the density is calculated in kg/m 3 . These values are entered in the test specification.
  • the distance between the clamps (75mm) and the distance of the long-travel transducer (50mm) are checked before the start of the test.
  • the test specimen is placed on the upper clamp and the force is tared.
  • the test specimen is clamped and the test is started.
  • the measurement is carried out with a test speed of 100 mm/min and a preload of 1 N.
  • the tensile strength a max (given in MPa) is calculated using Equation (1), it is the maximum stress that can be identical to the stress at break .
  • the elongation at break e (specified in %) is calculated using equation (2).
  • Three specimens per material are tested. The average of the three measurements is given. If the test specimen tears outside the marked area, this is noted. A repetition with another test body does not take place.

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

L'invention concerne un procédé de production de particules de mousse en élastomère thermoplastique expansé, qui comprend les étapes consistant à : mélanger une masse fondue d'élastomère thermoplastique à un agent d'expansion dans une extrudeuse ; presser la masse fondue d'élastomère thermoplastique mélangée à l'agent d'expansion à travers une plaque perforée dans une chambre de granulation ; fragmenter la masse fondue d'élastomère thermoplastique, mélangée à l'agent d'expansion et pressée à travers la plaque perforée, en granules individuelles, la chambre de granulation étant parcourue par un liquide dont la pression et la température sont choisies de telle sorte que les granules sont expansées à une valeur souhaitée dans le liquide par l'agent d'expansion contenu et se solidifient pour former des particules de mousse, ledit procédé comprenant au moins l'une des caractéristiques suivantes : (I) le liquide situé dans la chambre de granulation contient de la cire qui s'enrichit pendant la coupe et l'expansion dans la chambre de granulation sur la surface du granulat, (ii) après la séparation des particules de mousse contenues dans le liquide et leur séchage, une cire est appliquée sur les particules de mousse en élastomère thermoplastique expansé.
EP22711984.9A 2021-03-15 2022-03-10 Procédé de production de particules d'élastomère thermoplastique expansé Withdrawn EP4308355A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP21162613 2021-03-15
PCT/EP2022/056174 WO2022194665A1 (fr) 2021-03-15 2022-03-10 Procédé de production de particules d'élastomère thermoplastique expansé

Publications (1)

Publication Number Publication Date
EP4308355A1 true EP4308355A1 (fr) 2024-01-24

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EP22711984.9A Withdrawn EP4308355A1 (fr) 2021-03-15 2022-03-10 Procédé de production de particules d'élastomère thermoplastique expansé

Country Status (5)

Country Link
US (1) US20240182661A1 (fr)
EP (1) EP4308355A1 (fr)
CN (1) CN116981553A (fr)
TW (1) TW202248324A (fr)
WO (1) WO2022194665A1 (fr)

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5041251A (en) * 1989-07-27 1991-08-20 Eastman Kodak Company Pourable particles of normally tacky plastic materials and process for their preparation
DE4307648A1 (de) 1993-03-11 1994-09-15 Basf Ag Schaumstoffe auf Basis thermoplastischer Polyurethane sowie expandierbare, partikelförmige, thermoplastische Polyurethane, insbesondere geeignet zur Herstellung von Schaumstoff-Formkörpern
DE10356017A1 (de) * 2003-11-27 2005-07-07 Basf Ag Verfahren zur Herstellung expandierbarer Polyolefinpartikel mittels Kaltimprägnierung
EP1979401B1 (fr) 2006-01-18 2010-09-29 Basf Se Mousse a base de polyurethane thermoplastique
JP5248630B2 (ja) * 2008-03-13 2013-07-31 ビーエーエスエフ ソシエタス・ヨーロピア ポリオレフィン／スチレンポリマー混合物に基づく弾性成形フォームビーズ
EP2452969A1 (fr) * 2010-11-11 2012-05-16 Basf Se Procédé de fabrication de particules thermoplastiques extensibles par imprégnation postérieure
EP2836543B1 (fr) 2012-04-13 2020-03-04 Basf Se Procédé de production de granulés expansés
EP2671633A1 (fr) 2012-06-06 2013-12-11 Basf Se Procédé de transport de particules de polymère thermoplastiques moussées
TWI667285B (zh) * 2013-10-18 2019-08-01 德商巴斯夫歐洲公司 膨脹熱塑性彈性體之製造

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Publication number Publication date
WO2022194665A1 (fr) 2022-09-22
CN116981553A (zh) 2023-10-31
US20240182661A1 (en) 2024-06-06
TW202248324A (zh) 2022-12-16

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