Procedure for the devulcanization of scrap rubber and/or elastomers and apparatus therefor
20180251624 ยท 2018-09-06
Inventors
Cpc classification
C08J11/10
CHEMISTRY; METALLURGY
B29C48/767
PERFORMING OPERATIONS; TRANSPORTING
B29B7/488
PERFORMING OPERATIONS; TRANSPORTING
Y02W30/62
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
B29C2948/9238
PERFORMING OPERATIONS; TRANSPORTING
B29C2948/92876
PERFORMING OPERATIONS; TRANSPORTING
B29C2948/92714
PERFORMING OPERATIONS; TRANSPORTING
C08J2319/00
CHEMISTRY; METALLURGY
C08J2321/00
CHEMISTRY; METALLURGY
B29K2021/00
PERFORMING OPERATIONS; TRANSPORTING
B29B7/845
PERFORMING OPERATIONS; TRANSPORTING
B29B7/726
PERFORMING OPERATIONS; TRANSPORTING
B29B7/485
PERFORMING OPERATIONS; TRANSPORTING
B29B2017/0464
PERFORMING OPERATIONS; TRANSPORTING
B29B17/04
PERFORMING OPERATIONS; TRANSPORTING
B29B7/487
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
A procedure for the devulcanization of scrap rubber and/or elastomers and apparatus therefor. The abstract of the disclosure is submitted herewith as required by 37 C.F.R. 1.72(b). As stated in 37 C.F.R. 1.72(b): A brief abstract of the technical disclosure in the specification must commence on a separate sheet, preferably following the claims, under the heading Abstract of the Disclosure. The purpose of the abstract is to enable the Patent and Trademark Office and the public generally to determine quickly from a cursory inspection the nature and gist of the technical disclosure. The abstract shall not be used for interpreting the scope of the claims. Therefore, any statements made relating to the abstract are not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
Claims
1. A method of devulcanizing vulcanized material comprising cross-linked rubber or cross-linked elastomers, using a planetary roller extruder comprising a housing, a central spindle, and planetary spindles disposed between and configured to mesh with said central spindle and said housing, said method comprising the steps of: feeding vulcanized material into a feed zone of said planetary roller extruder; operating said planetary roller extruder by rotating said central spindle about its rotational axis, and thereby both rotating said planetary spindles about each of their rotational axes and revolving said planetary spindles about said central spindle; feeding vulcanized material from said feed zone into a first treatment zone; generating mechanical and thermal stress on said vulcanized material in said first treatment zone by kneading and/or crushing to begin devulcanization; feeding treated vulcanized material from said first treatment zone, through a dispersion ring, and to a second treatment zone, and generating additional mechanical and thermal stress on said treated vulcanized material by restricting movement of said vulcanized material through said dispersion ring; generating additional mechanical and thermal stress on said treated vulcanized material in said second treatment zone by kneading and/or crushing to further and/or complete devulcanization; and said step of generating mechanical and thermal stress on said vulcanized material in said first treatment zone comprising: (A) heating said vulcanized material in a heating zone, which heating zone comprises its own set of planetary rollers and temperature control; and/or (B) starting devulcanization in a start zone, which start zone comprises its own set of planetary rollers and temperature control.
2. The method according to claim 1, wherein the length of said heating zone and/or said start zone, relative to the diameter of the pitch circle the toothing on the inside of said housing, are as follows: TABLE-US-00005 Diameter Size Module length Module length of Pitch Circle Heating zone Start zone 50 to 70 mm 100 to 300 mm 100 to 300 mm 100 to 150 mm 250 to 600 mm 250 to 650 mm 170 to 250 mm 300 to 650 mm 300 to 650 mm 280 to 300 mm 320 to 800 mm 320 to 800 mm 350 mm 300 to 650 mm 300 to 650 mm 400 mm 320 to 800 mm 120 to 800 mm 400 mm 320 to 800 mm 320 to 800 mm 500 to 1000 mm 350 to 1000 mm 350 to 1000 mm.
3. The method according to claim 2, wherein said step of heating said vulcanized material in said heating zone comprises quickly raising the temperature of said vulcanized material to a starter temperature for devulcanization using a temperature control agent having a temperature of one of: (C) at least 300 C., (D) at least 320 C., and (E) at least 340 C.
4. The method according to claim 3, wherein said vulcanized material in said start zone exhibits the required starter temperature and after leaving said start zone exhibits a lower temperature.
5. The method according to claim 4, wherein said method further comprises selecting and setting a start temperature that is sufficiently high to be in a start range, and then reducing the selected temperature in steps until an optimal start temperature is reached.
6. The method according to claim 5, wherein said planetary roller extruder comprises a plurality of dispersion rings and a plurality of planetary roller modules, wherein each dispersion ring is associated with a corresponding planetary roller module, such that processing linked with the dispersion rings is carried out on said vulcanized material in a plurality of steps.
7. The method according to claim 6, wherein: each of said dispersion rings is disposed about said central spindle with space therebetween, such that slits are formed between said dispersion rings and said central spindle ro permit vulcanized material to pass through; the opening width of the slits is reduced with each processing step or with each planetary roller module, wherein: the opening width of a second dispersion ring compared to the opening width of a first dispersion ring is one of: at least 5% less, at least 10% less, or at least 15% less; the opening width of a third dispersion ring compared to the opening width of said second dispersion ring is one of: at least 5% less, at least 10% less, at least 15% less, or at least 20% less; and the opening width of a fourth dispersion ring compared to the opening width of said third dispersion ring is one of: at least 5% less, at least 10% less, at least 15% less, or at least 20% less; and said dispersion rings are exchangeable in order to permit modification of the opening width of said slits.
8. The method according to claim 7, wherein the lengths of said slits are defined by the thicknesses of said dispersion rings, which thicknesses are in the range of 1 to 25 mm, or are in the range of 3 to 20 mm, and the dispersion rings are exchangeable in order to permit modification of the lengths of said slits.
9. The method according to claim 8, wherein said slits comprise a conical shape, with an inlet conus and/or an outlet conus and/or with rounded edges and/or with a conical surface inclination, with respect to the central axis of said dispersion rings, in the range of: 1 to 45, 10 to 35, or 15 to 30.
10. The method according to claim 9, wherein: said central spindle comprises groove portions about which said dispersion rings are disposed; said dispersion rings are composed of halves or a plurality of segments; the outer surface of each of said groove portions is rounded or cylindrical; and said groove portions remain unchanged in the event of an exchange of dispersion rings.
11. The method according to claim 10, wherein some of said dispersion rings have different sizes and/or dimensions and/or shapes, wherein said different dispersion rings, on the side adjacent the housing, comprise a collar of constant thickness, and, on the side adjacent the central spindle, comprise a flange configured to engage with said groove portions, which flanges have different thickness.
12. The method according to claim 11, wherein said dispersion rings are configured to be placed between two planetary roller modules, and are configured to be arranged together with thrust rings of planetary roller modules in a single arrangement, in order to sufficiently strongly deform the vulcanized material being devulcanized as it passes through said slits.
13. The method according to claim 12, wherein said planetary roller modules have a length selected to permit a desired positioning of said dispersion rings.
14. The method according to claim 13, wherein: said central spindle has a modular construction; said central spindle comprises a rod and a plurality of sleeves that disposed on said rod; said sleeves are clamped against one another with contact surfaces that engage in one another with teeth; said sleeves comprise a groove configured to engage with a dispersion ring; each of said sleeves comprises a toothing on its periphery that is configured to mesh with said planetary spindles; and said sleeves are exchangeable to change said grooves.
15. The method according to claim 14, wherein one of said dispersion rings is disposed before said heating zone, and the opening width of said slit is sufficiently large to permit the vulcanized material to be pushed through but sufficiently small to promote strong deformation of the vulcanized material.
16. The method according to claim 15, wherein said method further comprises: controlling the temperature at said planetary roller modules using a temperature control medium, which temperature control medium comprises oil; and preventing ignition of said oil at temperatures over 350 C. using nitrogen.
17. The method according to claim 16, wherein said method further comprises controlling the temperature at said dispersion rings.
18. The method according to claim 17, wherein said method further comprises filling said planetary roller extruder with vulcanized material to a fill level of less than 80%, or less than 70%, or less than 50%.
19. The method according to claim 18, wherein said method further comprises an additional degassing of said vulcanized material after leaving said planetary roller extruder, wherein said vulcanized material is mechanically stressed at the end of said planetary roller extruder by an additional dispersion ring.
20. The method according to claim 19, wherein: said planetary roller modules in said heating zone and/or said start zone comprise standard spindles; said planetary roller modules in said second treatment zone comprise back-cut spindles and/or transport spindles and/or transversal mixing spindles for degassing; said method further comprises producing a devulcanized material having a Mooney viscosity of 20 to 60, or 30 to 50, or 35 to 45, as measured at a temperature of 100 C.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
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DESCRIPTION OF EXEMPLIFICATION OR EXEMPLIFICATIONS
[0125] The extrusion line according to
[0126] Sections 3a, 3b, 4, 5, 6 are planetary roller modules, examples of which may be seen in
[0127] Each planetary roller module is equipped with five planetary spindles, though different designs can have lower or higher numbers of planetary spindles for each module, depending on the feedstock or material to be processed. The number of planetary spindles has an influence on the fill level of the planetary roller modules. The lower the number of planetary spindles the greater cavities can be produced. The planetary spindles of the modules 4 and 5 are designed as back-cut spindles and evenly distributed on the periphery of the central spindle. Among the planetary spindles of the module 6, three planetary spindles are likewise designed as back-cut spindles. The other planetary spindles of module 6 are designed as transport spindles. The planetary roller modules 3a and 3b possess more planetary spindles than the other planetary roller modules, namely six. Moreover, the planetary spindles of the modules 3a and 3b are equipped with a standard toothing. The standard toothing causes a higher mechanical stress of the scrap rubber than the planetary spindles provided in the other modules, whose back-cut spindles are very conducive for the degassing and whose transport spindles are conducive for both the degassing as well as for generating a considerable conveying effect. The scrap rubber is very strongly rolled out into thin layers in the standard toothing. This intensifies the heat flow.
[0128] Among the planetary spindles in the planetary roller modules 4, 5, 6, three back-cut spindles each have the same length of 373 millimeters. In contrast, the other planetary spindles are longer. They are 399 millimeters long. The different lengths of the planetary spindles advantageously draw in the scrap rubber into the active zones of the spindles.
[0129] Planetary roller modules 3a and 3b on the other hand are provided with three planetary spindles of this length. The other three planetary spindles have a shorter length of 373 millimeters. The planetary spindles slide on customary thrust rings, which, in at least one exemplification, can be connected to the dispersion rings.
[0130] The dispersion ring for the module 3a is labeled 19, the dispersion ring for the module 3b is labeled 20, the dispersion ring for the module 4 is labeled 21, and the dispersion ring for the module 5 is labeled 22. Moreover, one other dispersion ring 36 is provided on the last module 6. An example of a dispersion ring 101 can be seen in
[0131] The modules 3b, 5, 6 are equipped with a degassing unit 30, 32, 35. The degassing units are formed by side arm extruders that extend perpendicular or substantially perpendicular to the associated modules. In at least one exemplification, the side arm extruders, according to the view in
[0132] In this regard the side arm extruder 30 is at a short distance from the dispersion ring 19, the side arm extruder 32 is at a short distance from the dispersion ring 21, the side arm extruder 35 is at a short distance from the dispersion ring 22.
[0133] Each side arm extruder is subjected to a negative pressure. During the degassing the side arm extruders are run empty, such that feedstock or processed material that is under high pressure in the extruder and tends to exit with the suctioned-off gas, is forced back again into the extruder.
[0134] In the exemplification, the scrap rubber, in finely divided form, is dosed into the feed part 2. The dosing unit is labeled 7, and the material inlet is labeled 40. At the material inlet there is also an opening 41, through which remaining material can be blown out when the line is shut down.
[0135] During the devulcanization process, the planetary roller modules 3, 4, 5 are temperature controlled with oil coolers 10a, 10b, 11, 12, 13.
[0136] The temperature control for the feed part 2 is labeled 14. A temperature control 15 is also provided for the central spindle, which is not visible in
[0137] When starting up, first oil is introduced into the feed part 2 by a pump 45 before scrap rubber is fed to the feed part 2. This prevents, restricts, and/or minimizes the moving extruder parts from running dry.
[0138] The scrap rubber introduced into the feed part 2 is subjected to mechanical deformation and stress by the screw of the feed part 2. This simultaneously heats the scrap rubber. In addition, the temperature control agent of the temperature control 15 is set for example to a temperature of 120 degrees Celsius. In other examples a higher or lower temperature can be used. The temperature control 15 is in one possible exemplification adjustable to 140 degrees Celsius.
[0139] The scrap rubber is pressed out of the feed part 2 into the module 3a that forms a heating zone. In the heating zone the scrap rubber is heated to a material-dependent start temperature for devulcanization. In one example, the start temperature is 310 degrees Celsius. For this the temperature control 10a of the module 3a is set to 330 degrees Celsius in the example. The scrap rubber is simultaneously intensively mixed and rolled out in the module 3a.
[0140] After the scrap rubber has been heated to the start temperature, it is pressed through the slit on the dispersion ring 19. After homogenization from the dispersion ring 19, the molecular chains of the scrap rubber are broken up to such an extent that sulfur can escape from the feedstock or processed material. The release of the sulfur is promoted by the intensive mixing and rolling out of the feedstock or processed material in the module 3b. The released, gaseous sulfur is simultaneously or substantially simultaneously suctioned off through the degassing unit 30.
[0141] The devulcanization of the feedstock is started in module 3b.
[0142] In order to achieve an adequate devulcanization the processing must or should be continued.
[0143] The feedstock or processed material is pressed out of module 3b into module 4. The feedstock or processed material passes the dispersion ring 20. In module 4 the feedstock or processed material is further processed and pressed through another dispersion ring 21. The thus-processed material is then further processed in module 5 and degassed.
[0144] After exiting the planetary roller module 5, the devulcanized scrap rubber is cooled down to 220 degrees Celsius in the planetary roller module 6 before exiting as a crumbly mass out of the extrusion line, and cooled down in a water cooler 16 to room temperature.
[0145] A water cooler 13 for the cooling is provided on the planetary roller module 6.
[0146] The feed part 2 is also equipped with a water cooler 14.
[0147] The cooling temperatures at the feed part and after the devulcanization are also material-dependent.
[0148] In the exemplification an internal cooling of the central spindle is also provided. The associated cooler 15, like the coolers 10, 11, 12, is an oil cooler and set to a temperature of 300 degrees Celsius.
[0149] The devulcanization is caused by the mechanical and thermal stressing of the scrap rubber in the extrusion line.
[0150] The dispersion rings 20, 21, 22 also contribute to the mechanical stress in the planetary roller modules 3, 4, 5.
[0151] In the exemplification the dispersion rings are arranged behind the thrust rings (not shown) in the machine direction of the scrap rubber through the unit.
[0152] In this regard, the inner diameter of the dispersion rings 20, 21, 22 is smaller than the external diameter of the central spindle. The dispersion rings 20, 21, 22 engage into the grooves (not shown) in the central spindle, such that the tooth gaps between the teeth of the central spindle are closed except for a narrow gap at the tooth base. The dispersion rings 20, 21, 22 are maintained between the corresponding ends of the planetary roller modules, such that the housing space around the central spindle is also closed and the scrap rubber is forced to pass through the narrow gap. The narrowing of the gap is material dependent and causes an extreme deformation and extreme mechanical stress of the feedstock.
[0153] In detail, the dispersion ring 20 is provided between the planetary roller modules 3 and 4, the dispersion ring 21 is provided between the planetary roller modules 4 and 5 and the dispersion ring 22 is provided between the planetary roller modules 5 and 6.
[0154] The dispersion rings 20, 21, 22 are clamped by clamping the cylindrical housing of the planetary roller modules 3, 4, 5, 6.
[0155] For this, the planetary roller modules 3, 4, 5, 6 possess on their ends typical flanges that are pushed against one another with clamping screws. The feed part 2 also possesses typical flanges. The feed part is clamped with these flanges on the one hand to the housing of the drive 1 and on the other hand with the planetary roller module 3.
[0156] For the dispersion rings 20, 21, 22, that in the exemplification engage into grooves of the central spindle, provision is made that these rings are composed of two halves in order to facilitate their mounting.
[0157] The mounting is mentioned below for the dispersion ring 20. The other dispersion rings 20, 21, 22 are mounted correspondingly.
[0158] After the feed part housing has been mounted, the central spindle with its end designed as a single screw is initially pushed into the feed part housing and coupled with the drive.
[0159] The housing of the planetary roller module 3 is then pushed over the central spindle and clamped with the feed part housing.
[0160] The planetary spindles of the planetary roller module 3 are then put in place. For this, the planetary spindles are rotatably pushed into their predefined position between the housing and central spindle. The position of the planetary spindles comprises an even distribution on the periphery of the central spindle and the already described toothing engagement of the planetary spindles with the inner toothing of the housing and the outer toothing of the central spindle.
[0161] After the planetary spindles have been put into position, the thrust ring for the planetary spindles is pushed over the central spindle and into a central opening of the housing end of the planetary roller module. The thrust ring has a wear resistant, hard metal coating in its contact area with the planetary spindles.
[0162] After the thrust ring has been put in position, the dispersion ring 20, comprising two halves, is moved to the thrust ring up against the machine. The halves are pushed at the same time into a groove of the central spindle. The dispersion ring is then centered with the help of a one-piece support ring that can be pushed over the central spindle and is centered in the same housing opening as the thrust ring in the planetary roller module 3. The dimensions of the support ring are such that it protrudes out of the end of the housing opening of the planetary roller module 3 and forms a centering means for mounting the following housing of the planetary roller module 4. The housing of the planetary roller module 4 is thus clamped with the housing of the planetary roller module 3 in the above described shape. This clamping simultaneously or substantially simultaneously clamps the thrust ring, the dispersion ring and the support ring.
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[0165] It should also be noted that the interior side or wall of the dispersion ring 114 is shown in
[0166] According to the present application, scrap rubber is devulcanized in a planetary roller extruder.
[0167] The following patents, patent applications, patent publications, and other documents, except of the exceptions indicated herein, are hereby incorporated by reference as if set forth in their entirety herein except for the exceptions indicated herein, as follows: DE 60004885 T2, published on Jun. 3, 2004, having applicant LEVGUM LTD; DE 909041, published on Apr. 12, 1954, having applicant METALLGESELLSCHAFT AG; DE 60008279 T2, published on Dec. 16, 2004, having applicant DSM IP ASSETS BV; DE 60215210 T2, published on Aug. 23, 2007, having applicant FULFORD GROUP INC; DE 60306089T2, published on Dec. 28, 2006, having applicant GOODYEAR TIRE & RUBBER; DE 60120804 T2, published on Jan. 11, 2007, having applicant BRIDGESTONE CORP; DE 601280412; WO2011/091966, published Aug. 4, 2011, having applicant RUST & MITSCHKE ENTEX; DE 69329245 T2, published on Mar. 29, 2001, having applicant UNIV AKRON AKRON; DE 69724239 T2, published on Jun. 9, 2004, having applicant TOYODA CHUO KENKYUSHO KK; DE 102009019846, published Nov. 11, 2010, having applicant H C CARBON GMBH; DE 102009013839, published on Sep. 23, 2010, having applicant RUST & MITSCHKE ENTEX; DE102008063036, published Jul. 1, 2010, having applicant TESA SE; DE 102008018686, published on Oct. 15, 2009, having applicant RUST & MITSCHKE ENTEX; DE 102007058174, published on Jun. 4, 2009, having applicant RUST & MITSCHKE ENTEX; DE102007050466, published on Apr. 23, 2009, having applicant RUST & MITSCHKE ENTEX; DE 102007041486, published on May 15, 2008, having applicant RUST & MITSCHKE ENTEX; DE 102007040645, published on Mar. 5, 2009, having applicant RUST & MITSCHKE ENTEX; DE 10 2004 048 440, published on Jun. 9, 2005, having applicant RUST & MITSCHKE ENTEX; U.S. Pat. No. 7,476,416, issued on Jan. 13, 2009, having applicant TYNAN JOHN K. JR; and EP 702739, published on Mar. 27, 1996, having applicant DEKONT TEKNIK AB.
[0168] One feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in a method of devulcanizing vulcanized material comprising cross-linked rubber or cross-linked elastomers, using a planetary roller extruder comprising a housing, a central spindle, and planetary spindles disposed between and configured to mesh with said central spindle and said housing, said method comprising the steps of: feeding vulcanized material into a feed zone of said planetary roller extruder; operating said planetary roller extruder by rotating said central spindle about its rotational axis, and thereby both rotating said planetary spindles about each of their rotational axes and revolving said planetary spindles about said central spindle; feeding vulcanized material from said feed zone into a first treatment zone; generating mechanical and thermal stress on said vulcanized material in said first treatment zone by kneading and/or crushing to begin devulcanization; feeding treated vulcanized material from said first treatment zone, through a dispersion ring, and to a second treatment zone, and generating additional mechanical and thermal stress on said treated vulcanized material by restricting movement of said vulcanized material through said dispersion ring; generating additional mechanical and thermal stress on said treated vulcanized material in said second treatment zone by kneading and/or crushing to further and/or complete devulcanization; and said step of generating mechanical and thermal stress on said vulcanized material in said first treatment zone comprising: (A) heating said vulcanized material in a heating zone, which heating zone comprises its own set of planetary rollers and temperature control; and/or (B) starting devulcanization in a start zone, which start zone comprises its own set of planetary rollers and temperature control.
[0169] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein the length of said heating zone and/or said start zone, relative to the diameter of the pitch circle the toothing on the inside of said housing, are as follows:
TABLE-US-00003 Diameter Size Module length Module length of Pitch Circle Heating zone Start zone 50 to 70 mm 100 to 300 mm 100 to 300 mm 100 to 150 mm 250 to 600 mm 250 to 650 mm 170 to 250 mm 300 to 650 mm 300 to 650 mm 280 to 300 mm 320 to 800 mm 320 to 800 mm 350 mm 300 to 650 mm 300 to 650 mm 400 mm 320 to 800 mm 120 to 800 mm 400 mm 320 to 800 mm 320 to 800 mm 500 to 1000 mm 350 to 1000 mm 350 to 1000 mm.
[0170] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said step of heating said vulcanized material in said heating zone comprises quickly raising the temperature of said vulcanized material to a starter temperature for devulcanization using a temperature control agent having a temperature of one of: (C) at least 300 C., (D) at least 320 C., and (E) at least 340 C.
[0171] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said vulcanized material in said start zone exhibits the required starter temperature and after leaving said start zone exhibits a lower temperature.
[0172] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said method further comprises selecting and setting a start temperature that is sufficiently high to be in a start range, and then reducing the selected temperature in steps until an optimal start temperature is reached.
[0173] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said planetary roller extruder comprises a plurality of dispersion rings and a plurality of planetary roller modules, wherein each dispersion ring is associated with a corresponding planetary roller module, such that processing linked with the dispersion rings is carried out on said vulcanized material in a plurality of steps.
[0174] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein: each of said dispersion rings is disposed about said central spindle with space therebetween, such that slits are formed between said dispersion rings and said central spindle ro permit vulcanized material to pass through; the opening width of the slits is reduced with each processing step or with each planetary roller module, wherein: the opening width of a second dispersion ring compared to the opening width of a first dispersion ring is one of: at least 5% less, at least 10% less, or at least 15% less; the opening width of a third dispersion ring compared to the opening width of said second dispersion ring is one of: at least 5% less, at least 10% less, at least 15% less, or at least 20% less; and the opening width of a fourth dispersion ring compared to the opening width of said third dispersion ring is one of: at least 5% less, at least 10% less, at least 15% less, or at least 20% less; and said dispersion rings are exchangeable in order to permit modification of the opening width of said slits.
[0175] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein the lengths of said slits are defined by the thicknesses of said dispersion rings, which thicknesses are in the range of 1 to 25 mm, or are in the range of 3 to 20 mm, and the dispersion rings are exchangeable in order to permit modification of the lengths of said slits.
[0176] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said slits comprise a conical shape, with an inlet conus and/or an outlet conus and/or with rounded edges and/or with a conical surface inclination, with respect to the central axis of said dispersion rings, in the range of: 1 to 45, 10 to 35, or 15 to 30.
[0177] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein: said central spindle comprises groove portions about which said dispersion rings are disposed; said dispersion rings are composed of halves or a plurality of segments; the outer surface of each of said groove portions is rounded or cylindrical; and said groove portions remain unchanged in the event of an exchange of dispersion rings.
[0178] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein some of said dispersion rings have different sizes and/or dimensions and/or shapes, wherein said different dispersion rings, on the side adjacent the housing, comprise a collar of constant thickness, and, on the side adjacent the central spindle, comprise a flange configured to engage with said groove portions, which flanges have different thickness.
[0179] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said dispersion rings are configured to be placed between two planetary roller modules, and are configured to be arranged together with thrust rings of planetary roller modules in a single arrangement, in order to sufficiently strongly deform the vulcanized material being devulcanized as it passes through said slits.
[0180] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said planetary roller modules have a length selected to permit a desired positioning of said dispersion rings.
[0181] One feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein: said central spindle has a modular construction; said central spindle comprises a rod and a plurality of sleeves that disposed on said rod; said sleeves are clamped against one another with contact surfaces that engage in one another with teeth; said sleeves comprise a groove configured to engage with a dispersion ring; each of said sleeves comprises a toothing on its periphery that is configured to mesh with said planetary spindles; and said sleeves are exchangeable to change said grooves.
[0182] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein one of said dispersion rings is disposed before said heating zone, and the opening width of said slit is sufficiently large to permit the vulcanized material to be pushed through but sufficiently small to promote strong deformation of the vulcanized material.
[0183] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said method further comprises: controlling the temperature at said planetary roller modules using a temperature control medium, which temperature control medium comprises oil; and preventing ignition of said oil at temperatures over 350 C. using nitrogen.
[0184] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said method further comprises controlling the temperature at said dispersion rings.
[0185] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method, wherein said method further comprises filling said planetary roller extruder with vulcanized material to a fill level of less than 80%, or less than 70%, or less than 50%.
[0186] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly In the method, wherein said method further comprises an additional degassing of said vulcanized material after leaving said planetary roller extruder, wherein said vulcanized material is mechanically stressed at the end of said planetary roller extruder by an additional dispersion ring.
[0187] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the method according to claim 19, wherein: said planetary roller modules in said heating zone and/or said start zone comprise standard spindles; said planetary roller modules in said second treatment zone comprise back-cut spindles and/or transport spindles and/or transversal mixing spindles for degassing; said method further comprises producing a devulcanized material having a Mooney viscosity of 20 to 60, or 30 to 50, or 35 to 45, as measured at a temperature of 100 C.
[0188] One feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in a process for devulcanization of crosslinked rubber and crosslinked elastomers, the molecular chains of which are destructible as far as the hydrocarbon molecules by mechanical and thermal stress, wherein the mechanical and thermal stress is generated in a planetary roller extruder, wherein the planetary roller extruder comprises a housing, planetary spindles and a central spindle, and the central spindle intermeshes with the planetary spindles and the planetary spindles intermesh with an internal toothing of the housing or with the internal toothing of a liner provided in the housing, such that a revolution of the central spindle causes the planetary spindles to rotate around the central spindle in the housing, wherein the planetary spindles of one extruder section slide with a facing surface at a thrust ring of this extruder section, wherein in the planetary roller extruder there is provided at least one dispersion ring that reduces the cross-sectional flow for the rubber and the elastomers more than does a thrust ring, wherein a separate heating zone with its own planetary roller module and its own temperature control is provided between the feed part and the devulcanization zone and/or a start phase with its own planetary roller module and its own temperature control is provided at the beginning of the devulcanization zone.
[0189] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the use of modularly constructed planetary roller extruders having the following module lengths
TABLE-US-00004 Module length Module length Size Heating zone Start phase 50 to 70 100 to 300 mm 100 to 300 mm 100 to 150 250 to 600 mm 250 to 650 mm 170 to 250 300 to 650 mm 300 to 650 mm 280 to 300 320 to 800 mm 320 to 800 mm (heavy-duty design) 350 300 to 650 mm 300 to 650 mm 400 320 to 800 mm 120 to 800 mm (heavy-duty design) 400 320 to 800 mm 320 to 800 mm 500 to 1000 350 to 1000 mm 350 to 1000 mm 500 to 1000 350 to 1000 mm 350 to 1000 mm (heavy-duty design)
[0190] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the temperature control agent in the heating zone exhibits a temperature of at least 300 degrees Celsius, in one possible exemplification at least 320 degrees Celsius and in yet another possible exemplification at least 340 degrees Celsius, such that the feedstock is very rapidly brought to the starter temperature for the devulcanization.
[0191] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the feedstock in the starter phase of the devulcanization zone exhibits the required and/or desired starter temperature and after leaving the starter phase exhibits a lower temperature.
[0192] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein on starting up the extruder firstly a start temperature is selected that is certainly in the start range and the temperature is reduced stepwise until the optimal start temperature is reached.
[0193] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of a plurality of dispersion rings, wherein each dispersion ring is associated with a planetary roller module, such that the processing linked with the dispersion rings is carried out on the feedstock in a plurality of steps.
[0194] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the opening width of the slit on the dispersion rings is reduced with each processing step, wherein in one possible exemplification the opening width on the second dispersion ring compared to the opening width on the first dispersion ring is at least 5%, in one possible exemplification at least 10%, in another possible exemplification at least 15% less, the third dispersion ring compared to the opening width on the second dispersion ring is at least 5%, in one possible exemplification at least 10%, in another possible exemplification at least 15% and in yet another possible exemplification at least 20% smaller, the third dispersion ring compared to the opening width on the second dispersion ring is at least 5%, in one possible exemplification at least 10%, in another possible exemplification at least 15% and in yet another possible exemplification at least 20% smaller, the fourth dispersion ring compared to the opening width on the third dispersion ring is at least 5%, in one possible exemplification at least 10%, in another possible exemplification at least 15% and in yet another possible exemplification at least 20% smaller, wherein for modifying the slit width the dispersion rings are exchangeable.
[0195] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of dispersion rings, whose slit length is defined by the thickness of the dispersion rings and is in one possible exemplification 1 to 25 millimeters, in another possible exemplification 3 to 20 millimeters, wherein the dispersion rings, in one possible exemplification for modifying the slit length are exchangeable.
[0196] A further another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of dispersion rings with a conical slit, in one possible exemplification with an inlet conus and/or an outlet conus and/or with rounded edges and/or with a conical surface inclination of 1 to 45 degrees, in another possible exemplification 10 to 35 degrees and in yet another possible exemplification 15 to 30 degrees to the central axis of the dispersion rings.
[0197] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of dispersion rings, wherein the dispersion rings of the devulcanization zone engage into a groove of the central spindle, wherein the dispersion rings are composed of halves or more segments, wherein the visible corners and edges in the cross section of the groove are in one possible exemplification rounded and/or wherein the groove, in the case where a dispersion ring is exchanged, remains unchanged.
[0198] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of different dispersion rings that on the side of the housing have a collar of constant or substantially constant thickness and on the side of the central spindle engage with a flange into the groove of the central spindle and may have flanges of different thickness.
[0199] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of dispersion rings that in a modular composition of an extrusion line can be arranged between two modules.
[0200] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of dispersion rings that can be arranged together with the thrust rings of planetary roller modules in a common construction, in order to sufficiently strongly deform the material being devulcanized as it passes through the slit.
[0201] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of modules with a length matched to the desired position of the dispersion rings.
[0202] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of a modularly constructed central spindle, wherein the central spindle comprises a rod, onto which various sleeves have been pushed and, wherein the sleeves are clamped against one another with the rod, in one possible exemplification with sleeves that on their contact surfaces engage in one another with teeth, wherein the sleeves possess a groove in the region of a dispersion ring, such that the dispersion ring can engage into the groove, wherein the sleeves, on their periphery, carry a toothing, with which they mesh with the planetary spindles, and wherein the sleeve is exchangeable with the area forming a groove.
[0203] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of a dispersion ring that is arranged before the planetary roller module of the heating zone and encloses the central spindle at a distance, wherein the distance is large enough in order that the material to be devulcanized can be pushed through and at the same time is small enough in order that the material to be devulcanized is strongly deformed as it passes through the gap.
[0204] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises oil as the temperature control agent that for temperatures above 350 degrees Celsius is employed under nitrogen.
[0205] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises temperature controlled dispersion rings.
[0206] Yet another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises a fill level of the extruder of less than 80%, in one possible exemplification less than 70%, in another possible exemplification less than 50%.
[0207] Still another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises an additional degassing of the feedstock after leaving the extruder, wherein the feedstock is mechanically stressed at the extruder end by an additional dispersion ring.
[0208] A further feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the use of planetary roller modules with standard spindles for the heating zone and/or for the start phase for the devulcanization and by the use of back-cut spindles and/or transport spindles and/or transversal mixing spindles for the degassing in the devulcanization zone.
[0209] Another feature or aspect of an exemplification is believed at the time of the filing of this patent application to possibly reside broadly in the process wherein the process comprises the production of a product with a Mooney viscosity of 20 to 60, in one possible exemplification 30 to 50, in another possible exemplification 35 to 45, measured at a temperature of 100 degrees Celsius.
[0210] The components disclosed in the patents, patent applications, patent publications, and other documents disclosed or incorporated by reference herein, may possibly be used in possible exemplifications of the present invention, as well as equivalents thereof.
[0211] The purpose of the statements about the technical field is generally to enable the Patent and Trademark Office and the public to determine quickly, from a cursory inspection, the nature of this patent application. The description of the technical field is believed, at the time of the filing of this patent application, to adequately describe the technical field of this patent application. However, the description of the technical field may not be completely applicable to the claims as originally filed in this patent application, as amended during prosecution of this patent application, and as ultimately allowed in any patent issuing from this patent application. Therefore, any statements made relating to the technical field are not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
[0212] The appended drawings in their entirety, including all dimensions, proportions and/or shapes in at least one exemplification of the invention, are accurate and are hereby included by reference into this specification.
[0213] The background information is believed, at the time of the filing of this patent application, to adequately provide background information for this patent application. However, the background information may not be completely applicable to the claims as originally filed in this patent application, as amended during prosecution of this patent application, and as ultimately allowed in any patent issuing from this patent application. Therefore, any statements made relating to the background information are not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
[0214] All, or substantially all, of the components and methods of the various exemplifications may be used with at least one exemplification or all of the exemplifications, if more than one exemplification is described herein.
[0215] The purpose of the statements about the object or objects is generally to enable the Patent and Trademark Office and the public to determine quickly, from a cursory inspection, the nature of this patent application. The description of the object or objects is believed, at the time of the filing of this patent application, to adequately describe the object or objects of this patent application. However, the description of the object or objects may not be completely applicable to the claims as originally filed in this patent application, as amended during prosecution of this patent application, and as ultimately allowed in any patent issuing from this patent application. Therefore, any statements made relating to the object or objects are not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
[0216] All of the patents, patent applications, patent publications, and other documents cited herein, and in the Declaration attached hereto, are hereby incorporated by reference as if set forth in their entirety herein except for the exceptions indicated herein.
[0217] The summary is believed, at the time of the filing of this patent application, to adequately summarize this patent application, However, portions or all of the information contained in the summary may not be completely applicable to the claims as originally filed in this patent application, as amended during prosecution of this patent application, and as ultimately allowed in any patent issuing from this patent application. Therefore, any statements made relating to the summary are not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
[0218] It will be understood that the examples of patents, patent applications, patent publications, and other documents which are included in this application and which are referred to in paragraphs which state Some examples of . . . which may possibly be used in at least one possible exemplification of the present application . . . may possibly not be used or useable in any one or more exemplifications of the application.
[0219] The sentence immediately above relates to patents, patent applications, patent publications, and other documents either incorporated by reference or not incorporated by reference.
[0220] The following issued U.S. patents and/or published U.S. patent applications are incorporated by reference herein: US 2015/0283728, published Oct. 8, 2015; US 2015/0043300, published Feb. 12, 2015; U.S. Pat. No. 9,193,106, issued Nov. 24, 2015; and U.S. Pat. No. 8,957,119, issued Feb. 17, 2015.
[0221] All of the patents, patent applications, patent publications, and other documents, except for the exceptions indicated herein, which were cited in the International Search Report dated Aug. 2, 2016, and/or cited elsewhere, as well as the International Search Report document itself, are hereby incorporated by reference as if set forth in their entirety herein except for the exceptions indicated herein, as follows: An introduction of the planetary roller extruder and areas of applications rubber devulcanization by Michael W Batton, Thomas J Malzahn, Michael Gerdon, and Ralf Quack, published in Proceedings of Antec 2015, 25 Mar. 2015, SPESociety of Plastics Engineers, pages 1-4; and EP 2164895 A1, published on Mar. 24, 2010, having applicant RHEIN CHEMIE RHEINAU GMBH.
[0222] The corresponding foreign and international patent publication applications, namely, Federal Republic of Germany Patent Application No. 10 2015 010 460, filed on Aug. 16, 2015, having inventor Harald RUST, and DE-OS 10 2015 010 460 and DE-PS 10 2015 010 460, and International Application No. PCT/EP2016/001015, filed on Jun. 16, 2016, having WIPO Publication No. WO 2017/028936 A1 and inventor Harald RUST, are hereby incorporated by reference as if set forth in their entirety herein, except for the exceptions indicated herein, for the purpose of correcting and explaining any possible misinterpretations of the English translation thereof. In addition, the published equivalents of the above corresponding foreign and international patent publication applications, and other equivalents or corresponding applications, if any, in corresponding cases in the Federal Republic of Germany and elsewhere, and the references and documents cited in any of the documents cited herein, such as the patents, patent applications, patent publications, and other documents, except for the exceptions indicated herein, are hereby incorporated by reference as if set forth in their entirety herein except for the exceptions indicated herein.
[0223] The purpose of incorporating the corresponding foreign equivalent patent application(s), that is, PCT/EP2016/001015 and German Patent Application 10 2015 010 460, is solely for the purposes of providing a basis of correction of any wording in the pages of the present application, which may have been mistranslated or misinterpreted by the translator, and to provide additional information relating to technical features of one or more exemplifications, which information may not be completely disclosed in the wording in the pages of this application.
[0224] Statements made in the original foreign patent applications PCT/EP2016/001015 and DE 10 2015 010 460 from which this patent application claims priority which do not have to do with the correction of the translation in this patent application are not to be included in this patent application in the incorporation by reference.
[0225] Any statements about admissions of prior art in the original foreign patent applications PCT/EP2016/001015 and DE 10 2015 010 460 are not to be included in this patent application in the incorporation by reference, since the laws relating to prior art in non-U.S. Patent Offices and courts may be substantially different from the Patent Laws of the United States.
[0226] All of the references and documents cited in any of the patents, patent applications, patent publications, and other documents cited herein, except for the exceptions indicated herein, are hereby incorporated by reference as if set forth in their entirety herein except for the exceptions indicated herein. All of the patents, patent applications, patent publications, and other documents cited herein, referred to in the immediately preceding sentence, include all of the patents, patent applications, patent publications, and other documents cited anywhere in the present application.
[0227] Words relating to the opinions and judgments of the author of all patents, patent applications, patent publications, and other documents cited herein and not directly relating to the technical details of the description of the exemplifications therein are not incorporated by reference.
[0228] The words all, always, absolutely, consistently, preferably, guarantee, particularly, constantly, ensure, necessarily, immediately, endlessly, avoid, exactly, continually, expediently, ideal, need, must, only, perpetual, precise, perfect, require, requisite, simultaneous, total, unavoidable, and unnecessary, or words substantially equivalent to the above-mentioned words in this sentence, when not used to describe technical features of one or more exemplifications of the patents, patent applications, patent publications, and other documents, are not considered to be incorporated by reference herein for any of the patents, patent applications, patent publications, and other documents cited herein.
[0229] The description of the exemplification or exemplifications is believed, at the time of the filing of this patent application, to adequately describe the exemplification or exemplifications of this patent application. However, portions of the description of the exemplification or exemplifications may not be completely applicable to the claims as originally filed in this patent application, as amended during prosecution of this patent application, and as ultimately allowed in any patent issuing from this patent application. Therefore, any statements made relating to the exemplification or exemplifications are not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
[0230] The details in the patents, patent applications, patent publications, and other documents cited herein may be considered to be incorporable, at applicant's option, into the claims during prosecution as further limitations in the claims to patentably distinguish any amended claims from any applied prior art.
[0231] While various aspects and exemplifications have been disclosed herein, other aspects and exemplifications are contemplated. The various aspects and exemplifications disclosed herein are for purposes of illustration and not intended to be limiting. Additionally, the words including, having, and variants thereof (e.g., includes and has) as used herein, including the claims, shall be open-ended and have the same meaning as the word comprising and variants thereof (e.g., comprise and comprises).
[0232] The purpose of the title of this patent application is generally to enable the Patent and Trademark Office and the public to determine quickly, from a cursory inspection, the nature of this patent application. The title is believed, at the time of the filing of this patent application, to adequately reflect the general nature of this patent application. However, the title may not be completely applicable to the technical field, the object or objects, the summary, the description of the exemplification or exemplifications, and the claims as originally filed in this patent application, as amended during prosecution of this patent application, and as ultimately allowed in any patent issuing from this patent application. Therefore, the title is not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
[0233] The abstract of the disclosure is submitted herewith as required by 37 C.F.R. 1.72(b). As stated in 37 C.F.R. 1.72(b): [0234] A brief abstract of the technical disclosure in the specification must commence on a separate sheet, preferably following the claims, under the heading Abstract of the Disclosure. The purpose of the abstract is to enable the Patent and Trademark Office and the public generally to determine quickly from a cursory inspection the nature and gist of the technical disclosure. The abstract shall not be used for interpreting the scope of the claims.
Therefore, any statements made relating to the abstract are not intended to limit the claims in any manner and should not be interpreted as limiting the claims in any manner.
[0235] The exemplifications of the invention described herein above in the context of the preferred exemplifications are not to be taken as limiting the exemplifications of the invention to all of the provided details thereof, since modifications and variations thereof may be made without departing from the spirit and scope of the exemplifications of the invention.