EP4161988A1 - Procédé de dé-vulcanisation d'un mélange de caoutchouc vulcanisé, dispositif pour la mise en oeuvre du procédé, ainsi qu'un mélange de caoutchouc et un pneu de véhicule, comportant un composant constitué du mélange de caoutchouc - Google Patents

Procédé de dé-vulcanisation d'un mélange de caoutchouc vulcanisé, dispositif pour la mise en oeuvre du procédé, ainsi qu'un mélange de caoutchouc et un pneu de véhicule, comportant un composant constitué du mélange de caoutchouc

Info

Publication number
EP4161988A1
EP4161988A1 EP21731920.1A EP21731920A EP4161988A1 EP 4161988 A1 EP4161988 A1 EP 4161988A1 EP 21731920 A EP21731920 A EP 21731920A EP 4161988 A1 EP4161988 A1 EP 4161988A1
Authority
EP
European Patent Office
Prior art keywords
range
rubber
vulcanized
rubber mixture
rubber particles
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.)
Pending
Application number
EP21731920.1A
Other languages
German (de)
English (en)
Inventor
Alexander Burkhart
Hilke Wolf
Konstantin Efimov
Thomas Völker
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.)
Continental Reifen Deutschland GmbH
Original Assignee
Continental Reifen Deutschland GmbH
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 Continental Reifen Deutschland GmbH filed Critical Continental Reifen Deutschland GmbH
Publication of EP4161988A1 publication Critical patent/EP4161988A1/fr
Pending legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/0026—Recovery of plastics or other constituents of waste material containing plastics by agglomeration or compacting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04—Disintegrating plastics, e.g. by milling
    • B29B17/0412—Disintegrating plastics, e.g. by milling to large particles, e.g. beads, granules, flakes, slices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • 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
    • 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
    • B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7476—Systems, i.e. flow charts or diagrams; Plants
    • B29B7/7495—Systems, i.e. flow charts or diagrams; Plants for mixing rubber
    • 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
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/885—Adding charges, i.e. additives with means for treating, e.g. milling, the charges
    • 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
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/90—Fillers or reinforcements, e.g. fibres
    • 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
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/94—Liquid charges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08C—TREATMENT OR CHEMICAL MODIFICATION OF RUBBERS
    • C08C19/00—Chemical modification of rubber
    • C08C19/08—Depolymerisation
    • 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
    • C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
    • C08J11/12—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by dry-heat treatment only
    • 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
    • C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
    • C08J11/18—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material
    • C08J11/28—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with organic material by treatment with organic compounds containing nitrogen, sulfur or phosphorus
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/01—Hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04—Disintegrating plastics, e.g. by milling
    • B29B2017/042—Mixing disintegrated particles or powders with other materials, e.g. with virgin materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B17/00—Recovery of plastics or other constituents of waste material containing plastics
    • B29B17/04—Disintegrating plastics, e.g. by milling
    • B29B2017/0424—Specific disintegrating techniques; devices therefor
    • 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
    • B29B7/40—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with single shaft
    • B29B7/42—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with single shaft with screw or helix
    • 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
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • 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
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2030/00—Pneumatic or solid tyres or parts thereof
    • 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
    • C08J2317/00—Characterised by the use of reclaimed rubber
    • 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
    • C08J2319/00—Characterised by the use of rubbers not provided for in groups C08J2307/00 - C08J2317/00
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

Definitions

  • the invention relates to a method for devulcanizing a vulcanized rubber mixture.
  • the invention also includes an apparatus for performing the
  • old rubber One of the previous approaches to recycling old rubber, also known as old rubber, is the devulcanization of the old rubber that has already been vulcanized.
  • CN 105729755 discloses a multi-stage process for the production of injection molds
  • CN 102250381 B discloses a two-screw desulphurisation system for rubber, consisting of: a cylinder body, a double screw and a heating device in the Cylinder body, the cylinder body with a feed connection, the double screw with a conveying part and with two or more shear areas that are separated from one another, and a screw transition part and a mixing part between two adjacent shear areas (see. Claim 1).
  • US 2015148435 discloses a method for devulcanizing a vulcanized rubber, comprising the following steps: a) providing at least one vulcanized rubber; b) grinding the vulcanized rubber into aggregates; c) to knead the ground rubber obtained from step b) at a low shear rate between 100 1 / s and 500 1 / s so that it is homogenized in the size of the aggregates and in the temperature; d) Achieving a non-degenerating mechanical treatment on the kneaded rubber obtained from step c), a high shear rate between 1,000 1 / s and 1,000,000 1 / s being used (cf. claim 1).
  • EP 1201390 discloses a method for devulcanizing crosslinked rubber, consisting of a reclaim stage of crosslinked rubber by applying shear stress to the crosslinked rubber, the maximum pressure in the reclaim stage being 1.5 MPa or more (cf. claim 1 ).
  • WO 2014/032818 A1 describes that the rubber mixture produced according to the method disclosed in WO 2014/032818 A1 shows faster aging of the vulcanizates produced from the rubber mixtures compared to reference and comparative measurements (cf. values of the elongation at break before and after aging in Table 2 of WO 2014/032818 A1).
  • One object on which the invention is based is to provide a method for devulcanizing a vulcanized rubber mixture with which a devulcanized rubber can be produced from which a rubber mixture with improved properties and / or without the disadvantages known from the prior art is formed .
  • step C) Extruding the vulcanized rubber particles produced in step B) in a twin screw extruder, so that a devulcanized rubber mixture is produced, with at least one regeneration reagent being added to the extruded rubber particles during the extrusion in step C), the one regeneration reagent at least one silane, at least one Plasticizers, at least one anti-aging agent, or mixtures thereof.
  • the regeneration reagent described above prevents shortening of the polymer chains of the rubber and / or at the same time changes the sulfur bridges of the vulcanized rubber particles so that they can be reused in a later further vulcanization if possible .
  • the latter point in particular leads to a longer one Service life in a tire or a technical rubber article with a rubber mixture in which a rubber that has been devulcanized according to the invention is used.
  • one regeneration reagent consisting of at least one silane, at least one plasticizer, at least one anti-aging agent, or mixtures thereof.
  • the expression “devulcanized” means that the processed, ie devulcanized, rubber mixture is less
  • the regeneration reagent comprising at least one plasticizer and at least one silane.
  • An anti-aging agent and at least one plasticizer and at least one silane comprises or
  • a resin an anti-aging agent, at least one plasticizer and at least one silane
  • the anti-aging agent preferably being selected from the group consisting of 2,6-di-tert-butyl-4-methylphenol (BHT), 2,2'-methylene -bis (4-methyl-6-tert-butyl-phenol), 2,2'-methylenebis (4-methyl-6-cyclohexyl-phenol), 2-mercaptobenzimidazole, N- (1,3-dimethylbutyl) - N'-phenyl-p-phenylenediamine (6PPD) and methyl-2-mercaptobenzimidazole.
  • BHT 2,6-di-tert-butyl-4-methylphenol
  • 2,2'-methylene -bis (4-methyl-6-tert-butyl-phenol) 2,2'-methylenebis (4-methyl-6-cyclohexyl-phenol
  • 2-mercaptobenzimidazole N- (1,3-dimethylbutyl) - N'-phen
  • the aging inhibitor improves the processability of a mixture comprising the rubber mixture devulcanized according to the invention.
  • the particularly preferred aging inhibitor 6PPD is used as an example of the aging inhibitors described above as preferred, which surprisingly lowers the Mooney viscosity of the rubber mixture devulcanized according to the invention without greatly influencing the elongation at break and the results of the fatigue-to-failure test.
  • the anti-aging agent 6PPD is also called "N- (1,3-dimethylbutyl) -N'-phenyl-p-phenylenediamine".
  • the regeneration reagent comprises one or more plasticizers or consists of one or more plasticizers, one or more plasticizers or each of the multiple plasticizers being particularly preferred
  • the regeneration reagent particularly preferably not comprising an anti-aging agent and no anti-aging agent added to the extruded rubber particles during the extrusion in step C) will.
  • An advantage of the aspect of the present invention described above is that a high proportion of aromatics in the plasticizer prevents shortening of the polymer chains during devulcanization of the vulcanized rubber particles and / or lowers the temperature in step C) of a method according to the invention.
  • the processability and / or service life of a tire or a technical rubber article is thus improved even further with the rubber mixture devulcanized according to the invention.
  • Plasticizers which are particularly advantageous for the present invention are described in the document EP 1493596 B1 in paragraphs [0007] to [0015].
  • the regeneration reagent comprises at least one silane and / or the total amount of silanes, which preferably comprise at least one disulfide or consist of one or more disulfides, in an amount in the range of less than 5% by weight, particularly preferably in an amount in Range of less than 1% by weight, very particularly preferably in an amount in the range of less than 0.1% by weight, in particular very particularly preferably no silane at all, in each case based on the total mass of the mass from in step C ) extruded vulcanized rubber particles and the mass of regeneration reagent added in step C).
  • An advantage of the aspect of the present invention described above is when the silane is used in the regeneration reagent from the genus of the disulfides. These are particularly suitable in a method according to the invention, for example in comparison with tetrasulfides.
  • a regeneration reagent with silanes is particularly advantageously used in a process according to the invention, the silanes having a total amount of regeneration reagent 40 to 100% by weight of disulfides, particularly preferably 55 to 85% by weight of disulfides and very particularly preferably 60 to 80% by weight Have disulfides.
  • Such a mixture is available, for example, under the trade name Si 266® from Evonik, which is described, for example, in DE 102006004062 A1.
  • Rubber particles is entered, based on the total mass of the vulcanized rubber particles extruded in step C), preferably 0.1 to 1 kWh / kg, and / or
  • the temperature of the vulcanized rubber particles is in the range from 50 to 200.degree. C., preferably in the range from 75 to 180.degree. C., particularly preferably in the range from 110 to 150.degree.
  • An advantage of the above-described aspect of the present invention is that if the above-described upper limits are adhered to, an even longer service life of a tire or a technical rubber article with the rubber mixture devulcanized according to the invention results.
  • the regeneration reagent has a surprisingly good effect in the temperature range. It is assumed that the regeneration reagent is distributed particularly well in the temperature range and thus traps radicals.
  • step D) occurring after step C) the devulcanized rubber mixture is kept at a temperature of 50 ° C. to 150 ° C., preferably from 100 ° C. to 150
  • the devulcanized rubber mixture preferably being heated to a temperature of 50 ° C to 150 ° C, preferably from 100 ° C to 150 ° C.
  • One advantage of the above-described aspect of the present invention is that if the above-described upper limits are adhered to, an even longer service life of a tire or a technical rubber article with the rubber mixture devulcanized according to the invention results.
  • a filter unit described above comprising a sieve and / or a perforated plate can be used directly after the twin screw extruder or directly after the further kneading unit and thus a rubber mixture filtered through this filter unit is an even better one Has processability.
  • the screw speed of the screws of the twin screw extruder during the extrusion in step C) being at least mainly in the range from 10 to 500 elm revolutions per minute, preferably in the range from 100 to 300 elm revolutions per minute.
  • Two screw extruders are extruded with a shear rate of less than 300 s 1 , preferably with a shear rate in the range from 1 s 1 to 100 s 1 , preferably in the range from 10 s 1 to 80 s 1 , the shear rates particularly preferably measured only on the screw elements which conveying elements are, and / or
  • the temperature of the vulcanized rubber particles is less than 200 ° C. and a devulcanized rubber mixture with a temperature of over 100 ° C. is formed, the two-screw extruder preferably having a length of less than 60D.
  • An advantage of the above-described aspect of the present invention is that if the above-described upper limits are adhered to, an even longer service life of a tire or a technical rubber article with the rubber mixture devulcanized according to the invention results.
  • the regeneration reagent has a surprisingly good effect in this temperature range. It is assumed that the regeneration reagent is distributed particularly well in the temperature range and thus traps radicals.
  • the expression “in an extruder with a shear rate in the range from X to Y” means that the shear rate is in the range from X to Y over all screw segments of the extruder.
  • the shear rate of a screw segment of an extruder is calculated using the following formula:
  • the vulcanized rubber particles resulting in step B) have a maximum particle diameter of 100 mm and / or
  • the proportion of the comminuted rubber particles resulting in step B) which passes through a sieve of 44 mesh in a sieve test according to the Japanese industrial standard JIS P-8207, comprises at least 50% by weight of the total mass of comminuted rubber particles resulting in step B), preferably at least 80% by weight of the total mass of comminuted rubber particles resulting in step B).
  • An advantage of the above-described aspect of the present invention is that the rubber particles produced in this way result in a particularly long service life of a tire or a technical rubber article with the rubber mixture devulcanized according to the invention and / or improved processability of the rubber mixture devulcanized according to the invention. This does not apply in particular if the vulcanized rubber particles resulting in step B) have a maximum particle diameter of more than 100 mm.
  • the average particle diameter of the rubber particles resulting in step B) being in the range from 0.01 mm to 50 mm, preferably in the range from 0.1 mm to 20 mm.
  • An advantage of the above-described aspect of the present invention is that the rubber particles produced in this way result in a particularly long service life of a tire or a technical rubber article with the rubber mixture devulcanized according to the invention and / or improved processability of the rubber mixture devulcanized according to the invention.
  • a method as described above comprising the following steps is particularly preferred:
  • step C) Extruding the vulcanized rubber particles produced in step B) in a two-screw extruder with an extruder barrel with a length of less than 60D, so that a devulcanized rubber mixture is produced, a regeneration reagent being added to the extruded rubber particles during the extrusion in step C), whereby the regeneration reagent comprises at least one plasticizer, each of the at least one plasticizer being an oil with a content of polycyclic aromatics in the range of 10 to 40 percent by weight, as determined by the IP346 method, and aromatic extracts treated from mild extraction solvents (MES) treated distillate (TD AE), and heavy naphthenic oils, the one regenerating reagent added during step C)
  • the regeneration reagent comprises at least one plasticizer, each of the at least one plasticizer being an oil with a content of polycyclic aromatics in the range of 10 to 40 percent by weight, as determined by the IP346 method, and aromatic extracts treated from mild extraction solvents (MES) treated distillate (TD
  • step C is added in an amount in the range from 10 to 0.1 wt .-%, based on the total mass of the mass of vulcanized rubber particles extruded in step C) and the mass of regeneration reagent added in step C), and does not comprise any silane, and
  • the temperature of the vulcanized rubber particles during the extrusion in step C) is in the range from 100 to 200 ° C., in a step E) occurring after step D) the devulcanized rubber mixture is heated to a temperature of 50 ° C. to 150 ° C.
  • the screw speed of the screws of the two-screw extruder is at least mainly in the range from 100 to 300 revolutions per minute
  • the vulcanized rubber particles produced in step B) are extruded in the two-screw extruder with a shear rate of less than 300 s 1 will
  • the vulcanized rubber particles resulting in step B) have a maximum particle diameter of 100 mm and the average particle diameter of the rubber particles resulting in step B) is in the range from 0.01 mm to 50 mm.
  • the invention also relates to a device for carrying out a method according to one of the preceding claims, comprising a two-screw extruder, preferably with a length of less than 60D.
  • a device is preferred as described above or as described above as preferred, the one two-screw extruder having a feed unit for supplying a regeneration reagent as described above or as described above as preferred, the supply unit being set up to deliver the regeneration reagent at one point seen in a horizontal cross-section of the upper half of the inner wall of the extruder cylinder of the one twin screw extruder, with the upper half of the inner wall of the extruder cylinder seen in the horizontal and perpendicular to the extrusion direction being particularly preferred, the half of the inner wall of the extruder cylinder, which is, for example, in a horizontally aligned extruder cylinder is further from the ground.
  • An advantage of the above-described aspect of the present invention is that the pressure fluctuations in the rubber mixture in the said two-screw extruder are reduced and thus the rubber mixture devulcanized according to the invention thus has the desired elongation at break and the resulting vulcanizate has the desired service life.
  • a device as described above or as described above as preferred is preferred, the device additionally comprising: - A further kneading unit connected downstream of the one twin screw extruder, which preferably comprises a single screw extruder and / or a gear pump and / or a mixer for producing rubber mixtures, and / or
  • a filter unit comprising a sieve and / or a perforated plate and / or
  • a particle comminution unit for comminuting a vulcanized rubber mixture into a granulate of vulcanized rubber particles with a maximum particle diameter of 100 mm and / or with an average particle diameter in the range from 0.1 mm to 20 mm.
  • An advantage of the above-described aspect of the present invention is that a filter unit described above comprising a sieve and / or a perforated plate can be used directly after the twin screw extruder or directly after the further kneading unit and thus a rubber mixture filtered through this filter unit can be processed even better compared to devices without the filter unit. This can be recognized in particular from the improved Mooney viscosity or the improved elongation at break after vulcanization of the filtered rubber mixture.
  • the device having a mixer downstream of a two-screw extruder for producing the extrudate of the rubber mixture comprising a two-screw extruder and a molding unit downstream of a mixer for molding an unvulcanized body tire component comprises, wherein the molding unit is preferably set up to shape and cut a rubber mixture produced by means of the mixer comprising a rubber mixture devulcanized by means of the twin screw extruder into an unvulcanized tire component, and the unvulcanized tire component is particularly preferably an unvulcanized body tire component.
  • a two-screw extruder with a horizontally aligned extruder barrel with a length of less than 60D having a feed unit for feeding a regeneration reagent as described above, wherein the feed unit is arranged to deliver the regeneration reagent at a point in a horizontal and to introduce the upper half of the inner wall of the extruder cylinder of a two-screw extruder, as seen in the cross section perpendicular to the direction of extrusion,
  • a mixer which is connected downstream of the one twin screw extruder, for producing a rubber mixture comprising the extrudate of the one twin screw extruder
  • the invention also relates to a use of a device as described above or as described above as preferred - for devulcanizing a vulcanized rubber mixture and or
  • an unvulcanized rubber mixture comprising a devulcanized rubber mixture as described above or as described above as preferred is preferably carried out with a device according to the invention as described above or as described above as preferred or as described above as particularly preferred, wherein during mixing in the one described above More rubbers and other rubber compound ingredients are added to the mixer.
  • the invention also relates to a use
  • a rubber mixture is devulcanized by a method as described above or as described above as being preferred, or devulcanized
  • the processability of the rubber mixture is particularly important in the manufacture of the body tire components, since body tire components are particularly filigree and therefore tear quickly. This applies accordingly to mixtures for side stripes or apex mixtures as well as to wing components of treads and the base mixtures of treads. Therefore, the present invention has a particularly great advantage in such tire components.
  • vulcanization takes place in a vulcanization form known to the person skilled in the art and in the known temperature ranges between 100.degree. C. and 200.degree.
  • the vulcanized tire component or the vulcanized manufactured technical rubber article preferably the manufactured unvulcanized or manufactured vulcanized body tire component of a pneumatic vehicle tire, at least in one spatial direction having a maximum extension of 100 mm , preferably in one spatial direction has a maximum extension of 10 mm, and / or an elongation at break at room temperature according to DIN 53504 in the range of 4535% to 490%, preferably in the range of 468% to 480%, and / or in the “Fatigue to failure ”according to ASTM D4482 at 106% elongation and room temperature, values in the range of over 205 150 kC are achieved, preferably values in the range of over 300 kC, particularly preferred values in the range of over 500 kC, very particularly preferably values in the range of over 1000 kC, in particular very particularly preferred values in the range of more than 1500 kC or of 15 00 kC to 2000 kC.
  • An advantage of the aspect of the present invention described above is that the values described above can only be achieved with a rubber mixture which comprises a rubber devulcanized according to the invention.
  • the values described above as preferred can in particular be achieved with a regeneration reagent which consists exclusively of a resin.
  • a rubber mixture produced as described in the above uses goes through the following process according to the invention for producing a vulcanized tire or a vulcanized technical rubber article, comprising the following steps:
  • step C) extruding the vulcanized rubber particles produced in step B) in a two-screw extruder, preferably in a two-screw extruder according to FIG a device according to the invention as described above, so that a devulcanized rubber mixture is produced,
  • step D) feeding the devulcanized rubber mixture produced in step C) into a mixer, preferably into a mixer according to a device according to the invention described above,
  • step F) shaping and cutting the unvulcanized rubber mixture produced in step E) in a shaping unit, preferably in a shaping unit according to a device according to the invention described above, so that an unvulcanized tire component or an unvulcanized technical rubber article is produced,
  • step G vulcanizing the unvulcanized tire component produced in step F) or an unvulcanized technical rubber article produced in step F) in a vulcanization mold, optionally with further unvulcanized tire components, so that a vulcanized tire or a vulcanized technical rubber article is produced.
  • At least one regeneration reagent is added to the extruded rubber particles during the extrusion in step C), wherein the one regeneration reagent comprises at least one silane, at least one plasticizer, at least one anti-aging agent or mixtures thereof and preferably as described above in a method according to the invention or described as preferred is designed as described above in a method according to the invention described as particularly preferred and / or the rubber mixture components comprise at least one rubber, such as NR, BR, SBR, and a filler, such as silica or carbon black, the total amount of rubber preferably being 200 wt % to 500% by weight and / or the total amount of filler is preferably 100% by weight to 250% by weight, based in each case on the total amount of devulcanized rubber mixture supplied in step C).
  • the one regeneration reagent comprises at least one silane, at least one plasticizer, at least one anti-aging agent or mixtures thereof and preferably as described above in a method according to the invention or described as preferred is designed as described above in a method
  • the invention also relates to a rubber mixture which can be produced or produced
  • the vulcanized body tire component of a vehicle pneumatic tire being particularly preferably produced by vulcanization of an unvulcanized body tire component.
  • the invention also relates to a pneumatic vehicle tire or technical rubber article, comprising a component consisting of a rubber mixture as described above or as described above as preferred, wherein the component
  • - has a maximum extension of 100 mm at least in one spatial direction, preferably has a maximum extension of 10 mm in one spatial direction, and / or
  • - has an elongation at break at room temperature according to DIN 53504 in the range from 453% to 490%, preferably in the range from 468% to 480%, and / or
  • values in the range of over 205 kC were achieved, preferably values in the range of over 300 kC or from 300 kC to 5000 kC, particularly preferred values in the range of over 500 kC or from 500 kC to 4000 kC, very particularly preferred Values in the range from over 1000 kC or from 1000 kC to 2500 kC, in particular very particularly preferably values in the range from over 1500 kC or from 1500 kC to 2000 kC.
  • the pneumatic vehicle tire can also very generally be a vehicle tire and the component consisting of a rubber mixture as described above or, as described above as preferred, also be the component of a vehicle tire.
  • Vehicle tires and generally vulcanized rubber mixtures can, as already described above, be produced with new raw materials or with recycled raw materials, ie a new rubber or devulcanized rubber.
  • a devulcanized rubber After a devulcanized rubber has been incorporated into a rubber mixture, it can be identified afterwards, for example, in a component of a vehicle tire or generally in a vulcanized rubber mixture; it is irrelevant how the devulcanized rubber was produced.
  • the rubber can be identified with commercially available SEM microscopes with EDX function (these abbreviations stand for "Scanning Electron Microscopy (SEM) with Energy Dispersive X-Ray Analysis (EDX)"). Sufficient magnification in the sub-millimeter range should be used here.
  • devulcanized rubber can be distinguished from other primary and secondary particles or agglomerates, such as filler particles, so that a distinction can be made between vulcanized rubber mixtures with devulcanized rubber and vulcanized rubber mixtures without a devulcanized rubber.
  • vulcanized rubber compounds in vehicle tire components only vulcanized vehicle tire components with a rubber devulcanized according to the invention can have the elongations at break as described above for a vulcanized rubber mixture or a vehicle tire and / or the "fatigue to failure" values as described above for a vulcanized rubber mixture or a vehicle tire in the specified or preferred Achieve specified areas.
  • the person skilled in the art can thus distinguish vehicle tires according to the invention, in particular pneumatic vehicle tires according to the invention, from vehicle tires not according to the invention, in particular pneumatic vehicle tires not according to the invention.
  • the results were determined based on the ASTM D4482 method at 106% elongation and room temperature. The results are given in the unit kilo cycles (kC for short).
  • old truck tires were crushed in a particle crushing unit to form granules of vulcanized rubber particles with a maximum particle diameter of 100 mm and an average particle diameter in the range from 0.1 mm to 20 mm.
  • the devulcanizates according to the invention were produced from these granules in a two-screw extruder with an extruder barrel with a horizontally aligned extruder barrel with a length of less than 60D, the one two-screw extruder having a feed unit for supplying a regeneration reagent and the regeneration reagent at a point above the Extruder barrel was inserted vertically down into the extruder barrel of a two screw extruder.
  • the process for devulcanizing the vulcanized rubber particles produced comprised the following step C):
  • step C) extruding the vulcanized rubber particles produced in a twin-screw extruder with an extruder barrel with a length of less than 60D, wherein during the extrusion in step C) an amount of regeneration reagent according to Table 1 is added to the extruded rubber particles, the regeneration reagent
  • the screw speed of the screws of the twin screw extruder during the extrusion in step C) is 200 elm revolutions per minute and the vulcanized rubber particles during the extrusion in step C) in the twin screws -extruder are extruded at a shear rate of less than 300 s 1 , during step C) the temperature of the vulcanized rubber particles is in the range from 140 to 160 ° C and in a temperature control step D) taking place after step C) the devulcanized rubber mixture to a temperature from 50 ° C to 150 ° C for 10 minutes.
  • the devulcanizates according to the invention and not according to the invention were each mixed with further ingredients according to Table 2 below in a mixer in order to obtain rubber mixtures VB1, EB1 and EB2 according to the invention and not according to the invention.
  • the rubber mixtures obtained in this way were then used VB1, EB1 and EB2 are cut in a molding unit into a cut, unvulcanized test component and then vulcanized into a test component.
  • the molding unit comprised an extruder with a front and end template for molding an unvulcanized component and a downstream cutting unit for cutting the unvulcanized component into the intended shape to test the elongation at break or the values for "fatigue-to-failure".
  • the vulcanizates of the rubber mixtures EB1 and EB2, which contain the devulcanizates E1 and E2 according to the invention have much higher and thus much better values in the fatigue-to-failure test than rubber mixtures such as VB1, which derive from the Contain prior art known devulcanizate VI. Even after 2 million cycles (i.e.> 2000 kC), no cracks that would have led to the test being aborted could be detected. This is an unexpected technical effect. This is particularly unexpected because the values when measuring the elongation at break differ only minimally from one another.
  • the rubber mixtures BEI and BE2 show a comparatively higher Mooney viscosity compared to the mixture VB1.
  • the Mooney viscosity shows in As a rule, the rubber mixtures are easier to process and the process reliability increases with the mixtures according to the invention.

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Abstract

La présente invention se rapporte à un procédé de dé-vulcanisation d'un mélange de caoutchouc vulcanisé, comprenant les étapes suivantes : A) utilisation ou fabrication d'un mélange de caoutchouc vulcanisé ; B) réduction du mélange de caoutchouc vulcanisé en un matériau granulaire constitué de particules de caoutchouc vulcanisé ; C) extrusion des particules de caoutchouc vulcanisé obtenues à l'étape B) dans une extrudeuse double vis, de telle sorte qu'un mélange de caoutchouc dé-vulcanisé est produit, pendant l'extrusion à l'étape C), au moins un réactif de régénération étant ajouté aux particules de caoutchouc extrudées, le réactif de régénération comportant au moins un silane, au moins un plastifiant, au moins un agent de protection contre le vieillissement ou des mélanges de ces derniers. L'invention se rapporte également à un dispositif pour la mise en œuvre du procédé, aux utilisations du dispositif, ainsi qu'à un mélange de caoutchouc et à un pneu de véhicule ou à un article de caoutchouc technique, comportant un composant constitué du mélange de caoutchouc.
EP21731920.1A 2020-06-08 2021-05-31 Procédé de dé-vulcanisation d'un mélange de caoutchouc vulcanisé, dispositif pour la mise en oeuvre du procédé, ainsi qu'un mélange de caoutchouc et un pneu de véhicule, comportant un composant constitué du mélange de caoutchouc Pending EP4161988A1 (fr)

Applications Claiming Priority (2)

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DE102020207121.7A DE102020207121A1 (de) 2020-06-08 2020-06-08 Verfahren zur Devulkanisation einer vulkanisierten Kautschukmischung, Vorrichtung zur Durchführung des Verfahrens und Verwendungen der Vorrichtung sowie Kautschukmischung als auch Fahrzeugluftreifen oder technischer Gummiartikel, umfassend ein Bauteil aus der Kautschukmischung
PCT/DE2021/200073 WO2021249593A1 (fr) 2020-06-08 2021-05-31 Procédé de dé-vulcanisation d'un mélange de caoutchouc vulcanisé, dispositif pour la mise en œuvre du procédé, ainsi qu'un mélange de caoutchouc et un pneu de véhicule, comportant un composant constitué du mélange de caoutchouc

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DE102022204351A1 (de) 2022-05-03 2023-11-09 Continental Reifen Deutschland Gmbh Vulkanisierbare Kautschukmischung und daraus herstellbares Kautschukprodukt
DE102022213983A1 (de) 2022-12-20 2024-06-20 Continental Reifen Deutschland Gmbh Vulkanisierbare Kautschukmischung, Vulkanisat und Kautschukprodukt

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WO2000074914A1 (fr) 1999-06-08 2000-12-14 Kabushiki Kaisha Toyota Chuo Kenkyusho Procede de recuperation de caoutchouc reticule
US6590042B1 (en) * 2000-10-06 2003-07-08 Ying Tang Recycled rubber processing and performance enhancement
JP2004315766A (ja) * 2003-02-28 2004-11-11 Yokohama Rubber Co Ltd:The 加硫ゴムの分解方法および分解ゴム組成物
US7193004B2 (en) 2003-06-30 2007-03-20 The Goodyear Tire & Rubber Company Pneumatic tire having a component containing low PCA oil
DE102006004062A1 (de) 2006-01-28 2007-08-09 Degussa Gmbh Kautschukmischungen
IT1406769B1 (it) * 2010-08-05 2014-03-07 Maris Flli Spa Procedimento per il recupero e la de-vulcanizzazione di gomma
CN102250381B (zh) 2011-07-22 2013-09-18 常州大学 一种双螺杆橡胶脱硫的装置及方法
FR2991687B1 (fr) 2012-06-08 2014-06-06 Plymouth Francaise Sa Regeneration des caoutchoucs vulcanises
DE102012108096A1 (de) * 2012-08-31 2014-03-06 Continental Reifen Deutschland Gmbh Verfahren zur Regenerierung von schwefelvernetzten Gummivulkanisaten zu Regeneraten
LT6053B (lt) * 2012-10-18 2014-08-25 Devulco, Uab Devulkanizavimo modifikatorius regeneruotos gumos miltelių gamybai
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DE102017201503A1 (de) * 2017-01-31 2018-08-02 Continental Reifen Deutschland Gmbh Verfahren zur Herstellung einer Rohmaterialmischung, Verfahren zur Herstellung einer Kautschukmischung und Verfahren zur Herstellung eines Vulkanisats
CN107936331B (zh) * 2017-11-10 2020-10-02 北京化工大学 一种多阶螺杆连续脱硫制备再生橡胶的方法
NL2020302B1 (en) * 2018-01-22 2019-07-29 Kargro Recycling B V A method of devulcanizing a rubber vulcanizate
DE102019219372A1 (de) * 2019-12-11 2021-06-17 Continental Reifen Deutschland Gmbh Verfahren zur Devulkanisation einer vulkanisierten Kautschukmischung, Vorrichtung zur Durchführung des Verfahrens und die Verwendung der Vorrichtung zur Devulkanisation einer vulkanisierten Kautschukmischung

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WO2021249593A1 (fr) 2021-12-16
DE102020207121A1 (de) 2021-12-09
US20230212369A1 (en) 2023-07-06

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