IP Library Granted Patent US 12691624
Granted Patent B2
US 12691624 · App. 18/001,090 · Granted Jul 28, 2026

Method for the devulcanisation of a vulcanisaed rubber mixture, device for carrying out the method, as well as a rubber mixture and vehicle pneumatic tyre, comprising a component made of the rubber mixture

Inventors: Alexander Burkhart (Essen, DE); Hilke Wolf (Isernhagen, DE); Konstantin Efimov (Shanghai, CN); Thomas Völker (Seelze, DE)
Assignee: Continental Reifen Deutschland GmbH
B29C48/07B29B17/0412B29C48/40B60C1/00C08C19/08C08J11/12C08J11/28C08K5/01C08K5/18B29B2017/0424B29L2030/00C08J2317/00
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Quick Facts
Patent No.
US 12691624
App. No.
18/001,090
Filed
Dec 8, 2022
Granted
Jul 28, 2026
Kind
B2
Art Unit
1759
USPC
521/41
Abstract

The invention relates to a process for devulcanizing a vulcanized rubber mixture, comprising the following steps: A) providing or producing a vulcanized rubber mixture, B) comminuting the vulcanized rubber mixture into a granulate of vulcanized rubber particles, C) extruding the vulcanized rubber particles produced in step B) in a twin-screw extruder to form a devulcanized rubber mixture, wherein, during the extruding in step C) at least one regeneration reagent is added to the extruded rubber particles, wherein the regeneration reagent comprises at least one silane, at least one plasticizer, at least one aging stabilizer or mixtures thereof. The invention also comprises an apparatus for performing the method and the uses of the apparatus, and a rubber mixture and also a pneumatic vehicle tyre or a technical rubber article comprising a component composed of the rubber mixture.

Claims (75)

1 . A method for devulcanization of a vulcanized rubber mixture, the method comprising:

A) producing a vulcanized rubber mixture;

B) processing the vulcanized rubber mixture into a granulate of vulcanized rubber particles;

C) extruding the vulcanized rubber particles produced in B) in a twin-screw extruder to form a devulcanized rubber mixture;

wherein during the extruding:

at least one regeneration reagent is added to the rubber particles in the extruder, wherein the at least one regeneration reagent comprises at least one of at least one silane, at least one plasticizer, at least one aging stabilizer, or mixtures thereof;

the vulcanized rubber particles produced in step B) are extruded in the twin screw extruder at a shear rate of below 300 s −1 , and

the temperature of the vulcanized rubber particles is below 200° C. and the devulcanized rubber mixture is formed at a temperature of above 100° C.;

wherein the twin-screw extruder has a length of less than 60 D.

2 . The method of claim 1 , wherein the at least one regeneration reagent

comprises the at least one plasticizer and the at least one silane, or

comprises the at least one aging stabilizer and the at least one plasticizer, or

comprises the at least one aging stabilizer and the at least one plasticizer and the at least one silane,

wherein, the at least one plasticizer includes an oil having a content of polycyclic aromatics in the range from 1% to 70% by weight, as determined by the IP346 method.

3 . The method of claim 1 , wherein the at least one regeneration reagent added during step C)

is added in an amount in the range from 20% to 0.1% by weight, in each case based on the sum of the mass of vulcanized rubber particles extruded in step C) and the mass of regeneration reagent added in step C).

4 . The method of claim 1 , wherein adding at least one regeneration reagent during the extruding further includes introducing a specific energy input of 0.01 to 5 kWh/kg into the vulcanized rubber particles based on the total mass of the vulcanized rubber particles extruded in step C).

5 . The method of claim 1 , wherein the devulcanized rubber mixture produced by the extruding is pressed through a filter unit comprising a sieve and a perforated plate, wherein the devulcanized rubber mixture is at a temperature of 50° C. to 150° C. when pressing through the filter unit.

6 . The method of claim 1 ,

the vulcanized rubber particles produced in step B) are extruded in the twin screw extruder at a shear rate in the range from 1 s −1 to 100 s −1 .

7 . The method of claim 1 , wherein

the average particle diameter of the rubber particles resulting in step B) is in the range from 0.01 mm to 50 mm,

and/or

the proportion of the processed rubber particles resulting in step B) that passes through a 44 mesh sieve in a sieve test according to Japanese industrial standard JIS P-8207 is at least 50% by weight of the total mass of processed rubber particles resulting in step B),

wherein the vulcanized rubber particles resulting in step B) have a maximum particle diameter of 100 mm.

8 . The method according to claim 1 , wherein the at least one regeneration reagent includes at least one plasticizer.

9 . The method according to claim 1 , wherein none of the regeneration reagent added in step C) is silane.

10 . The method according to claim 9 , wherein the at least one regeneration reagent added in step C) is selected from the group consisting of at least one plasticizer;

wherein the at least one plasticizer includes an oil having a content of polycyclic aromatics of in the range from 10% to 40% by weight, as determined by the IP346 method, the oil selected from mild extraction solvents (MES), treated aromatic extracts of treated distillate (TDAE), and naphthenic oils.

11 . The method according to claim 9 , wherein

the vulcanized rubber particles produced in step B) are extruded in the twin-screw extruder at a shear rate of below 300 s −1 ,

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 regeneration reagent added during step C) is added in an amount in the range from 10% to 0.1% by weight based on the sum of the mass of vulcanized rubber particles extruded in step C) and the mass of regeneration reagent added in step C),

the temperature of the vulcanized rubber particles during the extruding in step C) is in the range from 100° C. to 200° C.

12 . The method according to claim 1 , wherein the at least one regeneration reagent includes at least one plasticizer, and the at least one plasticizer includes an oil having a content of polycyclic aromatics of in the range from 10% to 40% by weight, as determined by the IP346 method, the oil selected from mild extraction solvents (MES), treated aromatic extracts of treated distillate (TDAE), and naphthenic oils.

13 . The method according to claim 1 , wherein

the vulcanized rubber particles produced in step B) are extruded in the twin-screw extruder at a shear rate from 1 s −1 to 100 s −1 ,

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 at least one regeneration reagent added in step C) includes at least one plasticizer, the least one plasticizer including an oil having a content of polycyclic aromatics in the range from 10% to 40% by weight, as determined by the IP346 method, and selected from mild extraction solvents (MES), treated aromatic extracts of treated distillate (TDAE) and heavy naphthenic oils,

the regeneration reagent added during step C) is added in an amount in the range from 10% to 0.1% by weight based on the sum of the mass of vulcanized rubber particles extruded in step C) and the mass of regeneration reagent added in step C), and

wherein none of the regeneration reagent added in step C) is silane.

14 . A method for devulcanization of a vulcanized rubber mixture, the method comprising:

A) producing a vulcanized rubber mixture;

B) processing the vulcanized rubber mixture into a granulate of vulcanized rubber particles;

C) extruding the vulcanized rubber particles produced in B) in a twin-screw extruder to form a devulcanized rubber mixture;

wherein during the extruding, at least one regeneration reagent is added to the rubber particles in the extruder, wherein the at least one regeneration reagent comprises at least one of at least one silane, at least one plasticizer, at least one aging stabilizer, or mixtures thereof;

wherein none of the regeneration reagent added in step C) is silane,

wherein the at least one regeneration reagent includes at least one plasticizer,

wherein each of the at least one plasticizer is an oil having a content of polycyclic aromatics of in the range from 10% to 40% by weight, as determined by the IP346 method, the oil selected from mild extraction solvents (MES), treated aromatic extracts of treated distillate (TDAE), and naphthenic oils.

15 . The method according to claim 14 , wherein the at least one regeneration reagent added during step C) is added in an amount in the range from 20% to 1% by weight, in each case based on the sum of the mass of vulcanized rubber particles extruded in step C) and the mass of regeneration reagent added in step C).

16 . The method of claim 14 , wherein adding at least one regeneration reagent to the extruded further includes introducing a specific energy input of 0.01 to 5 kWh/kg into the vulcanized rubber particles based on the total mass of the vulcanized rubber particles extruded in step C).

17 . The method of claim 14 , wherein during the extruding

the vulcanized rubber particles produced in step B) are extruded in the twin screw extruder at a shear rate in the range from 1 s −1 to 100 s −1 , measured at the screw elements,

and

the temperature of the vulcanized rubber particles is below 200° C. and a devulcanized rubber mixture having a temperature of above 100° C. is formed,

wherein the twin-screw extruder has a length of less than 60 D.

18 . The method of claim 14 , wherein

the average particle diameter of the rubber particles resulting in step B) is in the range from 0.1 mm to 20 mm,

and/or

the proportion of the processed rubber particles resulting in step B) that passes through a 44 mesh sieve in a sieve test according to Japanese industrial standard JIS P-8207 is at least 50% by weight of the total mass of processed rubber particles resulting in step B),

wherein the vulcanized rubber particles resulting in step B) have a maximum particle diameter of 100 mm.

19 . A method for devulcanization of a vulcanized rubber mixture, the method comprising:

A) producing a vulcanized rubber mixture;

B) processing the vulcanized rubber mixture into a granulate of vulcanized rubber particles;

C) extruding the vulcanized rubber particles produced in B) in a twin-screw extruder to form a devulcanized rubber mixture;

wherein during the extruding, at least one regeneration reagent is added to the rubber particles in the extruder;

wherein the at least one regeneration includes at least one plasticizer and at least one aging stabilizer;

wherein the at least one plasticizer includes an oil having a content of polycyclic aromatics of in the range from 10% to 40% by weight, as determined by the IP346 method, the oil selected from mild extraction solvents (MES), treated aromatic extracts of treated distillate (TDAE), and naphthenic oils; and

wherein the at least one aging stabilizer is 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′-methylene-bis(4-methyl-6-cyclohexyl-phenol), 2-mercaptobenzimidazole, N-(1,3-dimethylbutyl)-N′-phenyl-p-phenylenediamine (6PPD) and methyl-2-mercaptobenzimidazole.

20 . The method according to claim 19 , wherein

the vulcanized rubber particles produced in step B) are extruded in the twin-screw extruder at a shear rate of below 300 s −1 ,

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 regeneration reagent added during step C) is added in an amount in the range from 10% to 0.1% by weight based on the sum of the mass of vulcanized rubber particles extruded in step C) and the mass of regeneration reagent added in step C),

wherein none of the regeneration reagent added in step C) is silane,

the temperature of the vulcanized rubber particles during the extruding in step C) is in the range from 100° C. to 200° C.