Smooth EPDM profiles with blends of reclaimed carbon and carbon black
Patent Information
- Application Number
- PCT/US2024/035382
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-06-28
- Filing Date
- 2024-06-25
- Publication Date
- 2025-02-13
AI Technical Summary
Reclaimed carbon (rC) from end-of-life tires is difficult to disperse in EPDM rubber matrices, leading to surface defects in EPDM profiles, making its commercial use in products like weatherstrips challenging due to inferior filler-rubber interaction and ash residue issues.
A method involving the creation of solid pellets by milling reclaimed carbon and virgin carbon black together, followed by wet pelletizing and drying, to achieve a blend that can be used in EPDM profiles, allowing for improved dispersion and reduced surface defects.
The method enables the production of EPDM profiles with significantly reduced surface defects and comparable filler properties to those using 100% virgin carbon black, making rC a more viable filler material.
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Figure US2024035382_13022025_PF_FP_ABST
Abstract
Description
SMOOTH EPDM PROFILES WITH BLENDS OF RECLAIMED CARBON ANDCARBON BLACKBACKGROUND OF THE INVENTION
[0001] The present invention relates to methods for making EPDM profiles with recovered carbon or reclaimed carbon (rC) and EPDM profiles produced thereby. The present invention further relates to methods of making solid pellets of rC and carbon black.
[0002] There is more and more demand and effort in the recycling of materials so as to avoid the materials being disposed of in waste fills and to avoid further depletion of natural resources.
[0003] End-of-life vehicle tires are frequently processed and reused in a wide range of end-use applications from playground equipment to concrete. However, it is desirable to recycle components of tires to obtain materials that can be combined with first-use materials to reduce the amount of new material required to produce new products.
[0004] There is a growing need for more sustainable materials and reduced carbon footprint in various industries, including the weatherstrip industry. Reclaimed carbon (rC) obtained via pyrolysis of end-of-life-tires can be used to improve the circular content of EPDM weatherstrip compounds. However, unlike virgin carbon black, rC can be quite difficult to disperse well in the rubber matrix due to its inferior filler rubber interaction and / or the ash residue and / or other reasons. The undispersed rC aggregates and ash residues result in obvious defects on the surface of extruded EPDM profiles, which are undesired by the automotive OEM and end users and essentially make the use of rC not commercially feasible. Therefore, it has been a challenge to develop high surface quality EPDM weatherstrips with rC. There is a need in the weatherstrip industry and in other industries to address these problems and provide solutions so that rC can be incorporated into products, such as rubber profiles, hoses, and diaphragms.
[0005] All of the patents and publications mentioned throughout are incorporated in their entirety by reference herein.SUMMARY OF THE INVENTION
[0006] A feature of the present invention is to provide methods that utilize reclaimed carbon in forming pellets.
[0007] An additional feature of the present invention is to provide the ability to utilize reclaimed carbon and yet not interfere with the ability to produce industry acceptable products, such as EPDM profiles.
[0008] A further feature of the present invention is to provide methods to make reclaimed carbon a more viable material for use as filler grade material in such applications as EPDM profiles and the like.
[0009] A still further feature of the present invention is to provide the ability for the reclaimed carbon to disperse well in a polymer matrix and / or reduce or avoid defects, such as surface defects, in EPDM profiles and the like due to large undispersed rC agglomerates.
[0010] Also, a feature of the present invention is to provide methods to process reclaimed carbon, so that the particles in combination, for instance, with virgin carbon black can have comparable filler properties, such as, but not limited to, acceptable dispersion compared to utilizing 100% virgin carbon black.
[0011] An additional feature of the present invention is to provide a solid pellet (e.g., co-pellet) that contains at least reclaimed carbon along with virgin carbon black.
[0012] To achieve these and other advantages, and in accordance with the purposes of the present invention, as embodied and broadly described herein, the present invention, in part, relates a method of making a solid pellet. The method includes the steps of feeding reclaimed carbon particles and / or pellets, and feeding virgin carbon black particles and / or pellets as separate feeds to a mill (the same mill), and then milling a) the reclaimed carbon particles and / or pellets and b) the virgin carbon black particles and / or pellets together to obtained a milled blend. The method further includes wet pelletizing the milled blend to obtain wet solid pellets and drying the wet solid pellets to obtain dry solid pellets.
[0013] The present invention further relates, in part, to a method of making an EPDM profile (e.g., a film). The method includes the steps of blending at least one EPDM polymer with a plurality of solid pellets to form an EPDM formulation, and extruding the EPDM formulation to form a profile(s). The solid pellets include at least a milled blend of reclaimed carbon particles and virgin carbon black particles.
[0014] Further the present invention relates, in part, to a solid pellet that includes at least a blend of reclaimed carbon particles and virgin carbon black. The reclaimed carbon particles can have a D90 in a range of from <10 microns to <20 microns, and the virgin carbon black particles can have a D90 in a range of from 0.30 micron to 1.0 micron.
[0015] It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are intended to provide a further explanation of the present invention as claimed.
[0016] The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate various features of the present invention and, together with the description, serve to explain the principles of the present invention.BRIEF DESCRIPTION OF THE DRAWING
[0017] FIG. 1 are magnified images of three extruded tapes. The A) first extruded tape is made using only virgin carbon black as the carbon black component, B) the second extruded tape is made using a powder blend of reclaimed carbon and virgin carbon black (10:90 wt ratio), and C) the third extruded tape is made using the solid pellet of the present invention (10:90 wt ratio of reclaimed carbon to virgin carbon black in the pellets).
[0018] FIG. 2 is a graph showing the surface defect counts on the extruded tapes shown in A), B), and C) of FIG. 1.
[0019] FIG. 3 is a bar graph showing the volume resistivity of the extruded tapes shown in A), B), and C) of FIG. 1
[0020] FIG. 4 is a diagram showing an example of a set-up in a factory for making the solid pellets of the present invention.
[0021] FIG. 5 is a graph showing the surface defect counts on the extruded tapes produced in Example 2.
[0022] The Figures are not to scale and are provided as simplified views and do not necessarily show all possible embodiments or components that can be present.DETAILED DESCRIPTION OF THE INVENTION
[0023] The present invention relates, in part, to a method of making a solid pellet. The method comprises, consists essentially of, consists of, or includes feeding a) reclaimed carbon particles and / or pellets and b) feeding virgin carbon black particles and / or pellets as separate feeds to a mill and then milling the reclaimed carbon particles and / or pellets and the virgin carbon black particles and / or pellets together to obtained a milled blend, and then wet pelletizing the milled blend to obtain wet solid pellets, and then drying the wet solid pellets to obtain dry solid pellets.
[0024] The solid pellet being made is a solid pellet that comprises, consists essentially of, consists of, or includes a combination of milled reclaimed carbon and milled virgin carbon black.
[0025] For purposes of the present invention, the term “virgin carbon black particles” and the term “reclaimed carbon particles” are used throughout at times, but it is to be understood that the either of or both of the particles being fed to the mill can optionally be in pellet form.
[0026] The feeding of the reclaimed carbon and the feeding of the virgin carbon black to the mill are controlled to achieve a desired weight amount of each component. In the mill, the reclaimed carbon can be present in an amount of from 1 wt% to 50 wt%, and the virgin carbon black can be present in an amount of from 50 wt% to 99 wt%, based on total weight of particles in the mill. As further examples, the reclaimed carbon can be fed such that the amount in the mill is an amount of from 5 wt% to 20 wt%, and the virgin carbon black are present in an amount of from 80 wt% to 95 wt%, based on total weight of particles in the mill, or the reclaimed carbon can be present in an amount of from 5 wt% to 15 wt%, and the virgin carbon black can be present in an amount of from 85 wt% to 95 wt%, based on total weight of particles in the mill, or the reclaimed carbon can be present in an amount of from 10 wt% to 15 wt%, and the virgin carbon black can be present in an amount of from 85 wt% to 90 wt%, based on total weight of particles in the mill, or any range based upon any two values described herein.
[0027] The reclaimed carbon and virgin carbon black can be in a dry state when fed to the mill for milling. The moisture content for each can be below 2 wt% based on the weight of the particles.
[0028] As an option, the moisture content for either one or both of the reclaimed carbon or virgin carbon black can be 2 wt% or higher.
[0029] As an option, the reclaimed carbon or the virgin carbon black or both can be in a wet state when fed to the mill for milling, e.g., 65 wt% to 90 wt% or 70 wt% to 85 wt%, or 70 wt% to 80 wt% moisture or aqueous or water content, based on the weight of the wet particles. The wet state can result in a slurry of one or both of the particles introduced into the mill.
[0030] The feeding of the reclaimed carbon and virgin carbon black to the mill can be at the same time or about the same time, or can be sequential or in any order. As an option, the feeds of the reclaimed carbon and virgin carbon black can be combined together prior to their introduction into the mill.
[0031] The milling can be any type of milling that has the ability to reduce the size of solid particles and / or deagglomerate the particles. The milling can be a dry milling. Or alternatively, the milling can be a wet milling. Examples of acceptable types of milling include, but art not limited to, hammer milling, pin milling, air classification milling, long gap milling, jet milling, or media milling. The mill utilized to achieve the milling is commercially available and the manufacturer settings on the mill can be used. For instance, the hammer mill can be obtained from such suppliersas Prater, Williams, Hippo, and Schutte. The particles can be subjected to one milling step or more than one milling step. If more than one milling step is used, each milling step can be same or different from each other with respect to milling type and / or one or more milling parameters (e.g., milling time).
[0032] As an option, in this method, a portion or all of the virgin carbon black can be fed directly from a carbon black production line or multiple lines. The carbon black production line (e g., carbon black plant or carbon black furnace) can be located adjacent to the mill(s) or elsewhere in the facility or be in an adjacent facility. When the virgin carbon black is fed directly from a carbon black production line(s), the virgin carbon black may have been produced recently (e.g., produced within 1 minute to 12 hours or more of being fed to the mill, or within 5 minutes to 6 hours, within 5 minutes to 3 hours, within 5 minutes to 1 hour, within 10 minutes to 30 minutes).
[0033] The virgin carbon black, for instance as a result of being recently produced, can have a particle temperature of from 25 deg C to 200 deg C, for example, from 100 deg C to 200 deg C. This particle temperature can be an average temperature (e.g., determined by measuring the temperature of 1 kg of virgin carbon black in a container).
[0034] The virgin carbon black fed into the mill can be any grade of carbon black. The carbon black can be furnace carbon black or other types of carbon black.
[0035] The virgin carbon black particles can be any ASTM grade of carbon black. The virgin carbon black can be or include ASTM N100 series — N900 series carbon blacks, for example N100 series carbon blacks, N200 series carbon blacks, N300 series carbon blacks, N500 series carbon blacks, for example, N550 carbon black, N600 series carbon blacks, N700 series carbon blacks, N800 series carbon blacks, or N900 series carbon blacks. Carbon blacks sold under the Regal®, Black Pearls®, Spheron®, Sterling®, and Vulcan® trademarks available from Cabot Corporation, the Raven®, Statex®, Furnex®, and Neotex® trademarks and the CD and HV lines available from Birla Carbon (Columbian Chemicals,) and the Corax®, Durax®, Ecorax®, and Purex® trademarks and the CK line and other carbon blacks available from Orion Engineered Carbons, and other fillers suitable for use in such applications as polymers, films, rubber or tire applications, may also be exploited for use with various embodiments. Carbon blacks may be chemically functionalized. Suitable chemically functionalized carbon blacks include those disclosed in WO 96 / 18688 and US2013 / 0165560, the disclosures of which are hereby incorporated by reference.
[0036] The virgin carbon black may have a statistical thickness surface area (STS A, ASTM Standard D6556) of at least about 15 m2 / g, for example, from about 15 m2 / g to about 240 m2 / g,e.g., from about 35 m2 / g to about 230 m2 / g, from about 50 m2 / g to about 200 m2 / g, from about 60 m2 / g to about 180 m2 / g, from about 100 m2 / g to about 200 m2 / g.
[0037] Carbon blacks having any of the above surface areas may additionally have a structure, as given by the oil adsorption number for the compressed carbon black (COAN, ASTM D3493), of from about 50 to about 115 mL / 100 g, for example, from about 65 to about 75 mL / 100 g, from about 60 to 95 mL / 100 g, from about 75 to about 85 mL / 100 g, from about 85 to about 95 mL / 100 g, from about 95 to about 105 mL / 100 g, or from about 105 to about 115 mL / 100 g.
[0038] Mixtures of any of these carbon blacks may be used as an option.
[0039] The reclaimed carbon (the starting reclaimed carbon that is fed into the mill) or rC, such as rC aggregates, are commercially available. Generally, the rC aggregates result from the pyrolysis of tires and / or other rubber materials that contained filler materials or reinforcement materials, such as carbon black. The rC is made primarily of carbon black that was used to reinforce rubber. The rC can contain organic volatiles. The rC can contain char. Preferably, the rC used, though not required, has volatiles and / or char that is below 5 wt%, or below 3 wt%, or below 1 wt% (such as from 0.1 wt% to 4.9 wt%) based on the weight of the rC. The rC can be processed reclaimed carbon where the reclaimed carbon has been processed to remove or substantially remove at least one macroscopic contaminant such as fabric or wire. The reclaimed carbon can be commercially available from such suppliers as Reoil Sp. z o.o., Scandinavian Enviro Systems AB, Pyrum Innovations AG, CBp Cyprus Ltd., or Bolder Industries. The rC can be in pellet form or non-pellet form.
[0040] The reclaimed carbon may be processed to remove macroscopic contaminants. For example, magnetic separation techniques known to those of skill in the art may be used to remove wires and other macroscopic metallic contaminants. Filters or screens may be used to remove fabric and other non-magnetic macroscopic contaminants.
[0041] Alternatively or in addition, the reclaimed carbon may be processed to remove ash, for example, by washing the reclaimed carbon with acid or by using an ion exchanger. Exemplary methods are described in US20150307714, CN101357758, and WO2021 / 005124, the contents of all of which are incorporated herein by reference.
[0042] As an example, the starting reclaimed carbon pellets can have a D50 of from 0.5 mm to 2 mm, such as from 1.0 mm to 1.5 mm. Other D50 sizes above or below this range can be utilized. The rC fed to the mill can be in pellet form. The rC fed to the mill can be in non-pellet form (aggregate form or particulate form). The rC fed to the mill can have a D90 (non-pellet form) of 10 microns or higher, or 20 microns or higher, as an example.
[0043] As an option, the rC being fed to the mill (whether in pellet form or non-pellet form or particulate form) can have a D50 that is no lower than 0.5 mm.
[0044] With regards to the wet pelletizing step, this step can comprise, consist essentially of, consist of, or include blending the milled blend with an aqueous solution and optionally at least one binder and then forming the wet solid pellets. The amount of aqueous solution can be such that about a 1 to 1 weight ratio (of liquid to milled blend) is achieved. This weight ratio can vary with respect to the liquid and / or with respect to the milled blend by ± 5% or ± 10% or ± 20%, depending, e.g., on the surface area of the various components. As an example, the wetting of the milled blend for pelletizing can create a wet cake or wet sand consistency.
[0045] To pelletize the milled blend of particles, in a mixer, a spray nozzle can wet the particles with a binding agent or binder, such as water, toluene, mineral oil, or the like. The mixer mixes the binding agent and particles into a substantially homogenous mixture that agglomerates (or clumps) into pellets. The pellets can then be dried to a particular moisture content, such as less than 2% or less than 1% by weight. By reducing the moisture content of the pellets, the method of the present invention can prevent introduction of undesired moisture into polymer or rubber mixing that can contribute to gas emissions (or off-gassing) that may be emitted.
[0046] Any densification or pelletization method known to those of skill in the art may be employed. For example, the methods of U.S. Pat. No. 2,065,371 to Glaxner may be employed. In general, the wet milled blend is formed into beads, which may then be optionally dried to reduce the water content to at most 1% to form blended carbon pellets. In addition to the water already present in the wet blended carbon mixture, a wide variety of binder additives are known to be useful in the wet pelletization process to further improve the handling characteristics of the resulting pellets. Such additives include but are not limited to hygroscopic organic liquids such as ethylene glycol, carbohydrates (e.g., sugar, molasses, soluble starches, saccharides, lignin derivatives), rosin, sulfonate and sulfate anionic surfactants, fatty amine ethoxylate nonionic surfactants, sodium ligno sulfonates, silanes, sucrose, alkyl succinimides, alkylated succinic esters, and polyethylene oxide-co-polydimethyl siloxane surfactants. Alternatively or in addition, the pellets need not be dried and may be used wet, in which case it may not be necessary to use a binder. For example, wet pellets may have a moisture content of 15-80 wt%, for example 40-60 wt%.
[0047] The size of the pellets formed can be any size. For instance, the average size of the pellets formed can be from about 1 mm to about 2 mm. The average size can be determined by measuring by mechanical filtration on sieves according to ASTM DI 514.
[0048] When a binder(s) is used, the amount of binder can be an amount of from 0 ppm to 4000 ppm or from 100 ppm to 4000 ppm or from 250 ppm to 3000 ppm or from 500 ppm to 3000 ppm or from 750 ppm to 2500 ppm or from 1000 ppm to 3000 ppm based on the total weight of the dry milled blend.
[0049] The milling of the particles can be such that the milled blend can have a multimodal particle distribution with the mode of the major peak of the carbon black from 50-200 nm, for example, from 100 to 175 nm, and the mode of the major peak associated with the milled reclaimed carbon from 4-10 microns, for example, from 4-6 microns, as measured by light scattering.
[0050] The milling of the combination of the reclaimed carbon and virgin carbon black can result in the reclaimed carbon being reduced in size to a larger extent than the virgin carbon black based on a comparison of the starting size of the reclaimed carbon and the starting size of the virgin carbon black. For example, from the milling, the reclaimed carbon can be reduced in size by at least 10%, at least 20%, at least 30%, at least 40%, at least 50%, at least 60%, at least 70%, at least 80%, at least 90% based on the starting average or D50 size of the starting reclaimed carbon. The virgin carbon black can be reduced in size by no more than 10%, or no more than 5%, or no more than 1%.
[0051] As an option, the reclaimed carbon particles are fed to the mill in the absence of a pre-grinding or pre-milling. Put another way, the reclaimed carbon particles are not subjected to any size reduction step prior to being fed to the mill. In this option, the reclaimed carbon is obtained, for instance, from a supplier (e.g., in bulk form, in tote bags or bulk containers or IBCs) and fed to directly to the mill or unloaded into a container and then fed into the mill.
[0052] As an option, the reclaimed carbon particles are fed to the mill with pre-processing that can include, but is not limited to, sieving or screening or wetting or grinding or pre-milling, or magnetic screening or any combinations thereof.
[0053] The feeding of particles can be done utilizing any device. Examples include, but are not limited to, loss-in-weight feeders or silos preferably with metering devices to meter out the amount of each feed. The particles metered, for instance, in this manner can then be combined with a conveying air stream by any means, such as with an eductor device, which can create suction through a venturi effect as the conveying air passes through the eductor. The particles can be fed by other air conveying operations. Other conveying devices can be used such as but not limited to, conveyer belts or auger feeds or other commercially available conveying devices known to those skilled in the art.
[0054] FIG. 4 provides one example of a factory set-up that can be used to make the pellets of the present invention. The set-up 1 can involve the virgin carbon black manufacturing part and the reclaimed carbon part. For the virgin carbon black manufacturing part, if the carbon black is made nearby and used after formation (without bagging etc..), the materials 3 used to form the carbon black can be fed by lines 5 to the carbon black reactor 7 along with burner fuel. Once the carbon black is formed and subjected to quenching, the carbon black can be conveyed to a filtering unit 9 along with air being introduced. Once filtered, conveying air 11, for instance, can be used to transport the carbon black to a feeder 25. On the reclaimed carbon side, the rC can be transferred to a feeder 13 and with conveying air 15 introduced, an eductor 17 can transfer the rC with air to a feeder 27. Each feeder 25 and 27 can be controlled by metering to introduced the desired amount of carbon black and rC to the mill 29 (e.g., a hammermill or grinder). After milling, the milled blend is transferred to a pelletizing and drying unit 31 and then fed (e.g., by an auger feed) 33 to units 35 and 37 for packaging and shipping.
[0055] The present invention further relates to the solid pellet formed from a method of the present invention.
[0056] The present invention in addition relates to a solid pellet that comprises, consists essentially of, consists of or includes a blend of reclaimed carbon and virgin carbon black. As an option, the solid pellet of the reclaimed carbon particles and the virgin carbon black particles can have a D50 in a range of from 0.5 mm to 2 mm. A D50 above or below this range is possible.
[0057] The reclaimed carbon particles and virgin carbon black are generally evenly distributed throughout the pellet. The distribution can be considered a homogeneous blend.
[0058] The details of the reclaimed carbon and the virgin carbon black are described above and apply equally here.
[0059] The solid pellets have a BET surface area, an ash % content, a density, and / or a moisture %. The properties of the solid pellet can be characterized by comparison to one or more of these properties to a solid pellet made from 100% of the same carbon black alone with no other differences (identified here as the ‘control pellet’). From such a comparison, the solid pellet of the present invention can have one or more of the following characteristics: a) The BET surface area of the solid pellet increases by 1% to 15% such as from 5% to 15% or from 10% to 15% compared to the control pellet; b) The ash content (ash%) increases from 5 to 15 times or from 10 to 15 times compared to the control pellet;c) The moisture content (wt%) is the same, or about the same, or within 5% or within 1% of the control pellet; d) The density (g / 1) increases by from 1% to 5% or from 2% to 5% compared to the control pellet; e) The ash content increases from 1 to 1.5 wt% for every 5 wt% of reclaimed carbon present in the solid pellet (e.g., a solid pellet with 0 wt% rC has about 0.15 to 0.2 %; a solid pellet with 5 wt% rC has about 1.2 to 1.6 %, and a solid pellet with a 10 wt% rC has about 2.2 to 3 %, and a solid pellet with a 15 wt% rC has about 3.3 to 4 %).
[0060] As indicated, the solid pellet of the present invention can further include a binder present. Examples of binders are provided earlier. The binder can be present in amount of from 1 ppm to 4000 ppm or from 50 ppm to 4000 ppm or from 100 ppm to 3,000 ppm.
[0061] As indicated, the solid pellet of the present invention can have an average size of from about 0.5 mm to about 2 mm or from about 1 mm to about 2 mm or sizes above or below this range.
[0062] The solid pellet of the present invention can have a moisture content of less than 2 wt%, or less than 1.5 wt%, or less than 1 wt%, or less than 0.5 wt% based on the weight of the solid pellet.
[0063] The solid pellet can have the reclaimed carbon particles present in an amount of from 1 wt% to 50 wt% (e.g., from 1 wt% to 45 wt%, from 1 wt% to 40 wt%, from 1 wt% to 35 wt%, from 1 wt% to 30 wt%, from 1 wt% to 25 wt%, from 1 wt% to 20 wt%, from 1 wt% to 15 wt%, from 1 wt% to 10 wt%, from 1 wt% to 5 wt%, from 2.5 wt% to 50 wt%, from 5 wt% to 50 wt%, from 10 wt% to 50 wt%, from 15 wt% to 50 wt%, from 20 wt% to 50 wt%, or any range based upon any two values described herein), where the wt% is based on the total weight of the pellet.
[0064] The virgin carbon black particles can be present in an amount of from 50 wt% to 99 wt% (e.g., from 50 wt% to 95 wt%, from 50 wt% to 90 wt%, from 50 wt% to 80 wt%, from 50 wt% to 70 wt%, from 50 wt% to 60 wt%, from 55 wt% to 99 wt%, from 60 wt% to 99 wt%, from 65 wt% to 99 wt%, from 70 wt% to 99 wt%, from 75 wt% to 99 wt%, from 80 wt% to 99 wt%, from 85 wt% to 99 wt%, from 90 wt% to 99 wt%, from 95 wt% from 99 wt% or any range based upon any two values described herein), where the wt% is based on the total weight of the pellet.
[0065] As a more specific example, the solid pellet can have the reclaimed carbon particles present in an amount of from 5 wt% to 20 wt%, and the virgin carbon black particles present in an amount of from 80 wt% to 95 wt%, based on total weight of the solid pellet, or the solid pellet can have the reclaimed carbon particles present in an amount of from 5 wt% to 15 wt%, and the virgincarbon black particles present in an amount of from 85 wt% to 95 wt%, based on total weight of the solid pellet.
[0066] The solid pellets of the present invention can have a pellet hardness of from about 30 grams to about 45 grams or from 35 to 45 grams, measured by ASTM D5230.
[0067] The present invention further relates to a method of making an EPDM profile (e.g., a film or weatherstripping). The method can comprise, consists essentially of, consists of, or include blending at least at least one EPDM polymer with a plurality of the solid pellets of the present invention to form an EPDM formulation, and extruding the EPDM formulation to form the profile.
[0068] Exemplary formulations can be as follows (with wt% based on total weight of the formulation):
[0069] EPDM polymer - from 15 wt% to 40 wt%.
[0070] Solid pellets of the present invention- from 20 wt% to 40 wt% (e.g., from 15 wt% to 40 wt% or from 20 wt% to 40 wt%, or from 25 wt% to 40 wt%) (based on total weight of the formulation).
[0071] Other components that can typically be present in an EPDM formulation include, but are not limited to: a) Inorganic fillers (e.g., calcium carbonate, talc, clay) in amounts of from 10 to 25 wt%; b) Vulcanizates (e.g., N-Cyclohexyl-2-benzothiazole sulfenamide zinc-dibenzyl-dithiocarbamate, sulfur) in amounts of from 1 to 4 wt%; c) Plasticizer (e.g., paraffinic oil) in amounts of from 10 to 30 wt%;Processing Aids (e.g., polyethylene glycol) in amounts of from 0.1 to 1 wt%;Desiccants (e.g., calcium oxide) in amounts of from 0.5 to 3 wt%.
[0072] The formulation can be mixed or combined together using any mixing device, such as a blender.
[0073] The formulation can be extruded to form a profile using any type of extruder such as, but not limited to, a cold feed extruder, a hot feed extruder, or co-extruder. The extruder can be a multi -zone extruder.
[0074] With the present invention, when the solid pellets of the present invention are used in the method to form an EPDM profile as compared to direct mixing of the same amount of virgin carbon black and reclaimed carbon separately in non-co-pellet form (same amount and same type of each), the number of surface defects on the profile can be decreased by at least 20%, at least 30%, at least 40%, at least 50%, at least 60%, or at least 70%. These results were considered unexpected and quite superior to the direct mixing of each component.
[0075] The present invention relates to EPDM profiles prepared with both crystalline and amorphous EPDM. For the purpose of the present disclosure, crystalline EPDM, including semicrystalline EPDM, includes EPDM having an ethylene content of at least 60% and a thermodynamic transition, for example, a melting point or a crystallization point, at a temperature of at least 30 deg C.
[0076] Without wishing to be bound by any theory, it is believed that the solid pellets of the present invention enable a more homogenous mixing and / or weaker interaction between the milled reclaimed carbon particles compared to direct non-co-pellet blends. The virgin carbon black can serve as a carrier of sorts for the reclaimed carbon and thus improve the dispersion of the reclaimed carbon in the polymer matrix, which can reduce the surface defects of the extruded profiles.
[0077] The present invention also relates to an EPDM profile having low surface defects. The surface defects are measured based on the test method set forth in the Examples. In the test, an EPDM profile is made by extruding to form a tape have a thickness of 1 mm. A 165 cm2section of the tape is analyzed to determine the surface defect count for various sizes of defects. With the present invention, the EPDM profile utilizing the pellets of the present invention in EPDM polymers having either a thermodynamic transition at a temperature less than 30 deg C or an ethylene content less than 60 wt%, for example, in the EPDM formulation as provided in Example 1, has one or more of the following surface defect counts:1) Surface Defect size 80 to 100 microns — a surface defect count of 250 or less, such as 100 to 250 or 100 to 230.2) Surface Defect size 100 to 125 microns — a surface defect count of 200 or less, such as 100 to 200 or 100 to 150.3) Surface Defect size 125 to 150 microns — a surface defect count of 100 or less, such as 25 to 100 or 25 to 80.4) Surface Defect size 150 to 200 microns — a surface defect count of 150 or less, such as 50 to 150 or from 50 to 125.5) Surface Defect size 200 to 250 microns — a surface defect count of 50 or less, such as 10 to 50 or 10 to 25.6) Surface Defect size greater than 250 microns — a surface defect count of 35 or less, such as 5 to 35 or 5 to 25.
[0078] Alternatively or in addition, with the present invention, the EPDM profile utilizing the pellets of the present invention in EPDM polymers having a thermodynamic transition at atemperature of at least 30 deg C and an ethylene content of at least 60 wt%, for example, in the EPDM formulation as provided in Example 2, has one or more of the following surface defect counts, counted as described above:1) Surface Defect size 80 to 100 microns — a surface defect count of 120 or less, such as from 50 to 120 or from 50 to 90.2) Surface Defect size 100 to 125 microns — a surface defect count of 70 or less, such as from 25 to 70 or from 25 to 40.3) Surface Defect size 125 to 150 microns — a surface defect count of 25 or less, such as 5 to 25 or 5 to 20.4) Surface Defect size 150 to 200 microns — a surface defect count of 25 or less, such as from 13 to 25 or from 13 to 22.5) Surface Defect size 200 to 250 microns — a surface defect count of 8 or less, such as from 3 to 8 or 3 to 6.6) Surface Defect size greater than 250 microns — a surface defect count of 11 or less, such as from 3 to 11 or from 3 to 10.
[0079] The number of surface defects is measured on extruded 1 mm thick tapes via an automatic optical inspection machine, for example, produced by manufacturers such as Pixargus, Suzhou Oi- Smart Technology Co., or OCS Optical Control Systems. The camera scans the surface of the profile and automatically recognizes and measures the defects as areas of contrast with the background with a line speed of lOmm / s, a measuring field width of 28 mm, and a pixel resolution of 7 microns. The scanned surface area for each profile is 165 cm2. With the present invention, the pellets of the present invention, for example, using the formulations in the Examples, can be further characterized as having the ability to achieve this property in EPDM profiles with respect to one or more or all of these surface defect properties.
[0080] Further, the present invention can further relate to an EPDM profile having one or more or all of these surface defect properties.
[0081] And further, the present invention relates to methods to achieve one or more or all of these surface defect properties utilizing the pellets of the present invention in the EPDM formulation which is then formed (e.g., extruded) into an EPDM profile.
[0082] With respect to any of these invention embodiments, one of the surface defect properties (either 1), 2), 3), 4), 5) or 6)) is obtainable, or two or more properties (e.g., 1) and 2), 1), 2) and 3), or 1), 2), 3), and 4), or 1), 2), 3), 4) and 5), or 2) and 3), or 3) and 4), or 4) and 5), or 5) and 6), orany other combinations (e.g., two of the properties l)-6), three of the properties l)-6), four of the properties l)-6),or five of the properties l)-6) or all six of the properties).
[0083] The EPDM material made using the pellets of the present invention can have the following characteristics and / or properties.
[0084] The EPDM can have an ethylene content that can range from 45 wt% to 85 wt%, such as from 50 wt% to 70 wt% (based on the weight of the EPDM material).
[0085] The neat EPDM polymer can have a Mooney viscosity of from 20 MU to 150 MU (ML1+4@125 deg C), such as from 40 to 100 MU and / or from 20 MU to 150 MU (ML1+8@150 deg C), such as from 30 to 90 MU.
[0086] The EPDM can have a diene content such as ethylidene norbomene (ENB), dicyclopentadiene (DCPD), and / or 1,4 - hexadiene (HD) of from 0.5 wt% to 10 wt%.
[0087] Alternatively or in addition, the EPDM material (e.g., cured profile) can have one or more of the following properties:Mooney viscosity (MLl+4@100C) = 40 to 100 MU (ASTM D1646);Hardness (Shore A) = 45 to 90 (ASTM D2240).100% Modulus (MPa)= 1 to 5 (ASTM D412, Method A).300% Modulus (MPa)= 4 to 12 (ASTM D412, Method A).Tensile Strength (MPa)= greater than or equal to 6 -12 or 6-10 (ASTM D412, Method A).Elongation at Break (%)= 250 to 550 (ASTM D412, Method A).Compression set (70 h @ 23 deg C)= 0 to 40. (ASTM D345 Method B) Compression set (22 h @ 70 deg C)= 0 to 55. (ASTM D395 Method B)
[0088] The particle size distribution may be measured using any appropriate method, for example, laser diffraction, known to those of skill in the art. Preferably, particle size distribution is measured using scanning electron microscopy, for example, the scanning electron microscopy method described in more detail in the examples. In brief, the particles are dispersed at a concentration of 0.2 wt% in water with 600 ppm of Triton X 100 surfactant at low speed and then stirred for 24 hours. The dispersion is diluted to an appropriate concentration, filtered onto a membrane filter, dried, sputter coated with a conductive material, and imaged. Imaging is conducted at high and low magnification to provide sufficient resolution to capture small particles while efficiently imaging large particles. Images are processed to minimize uneven image background, increase particle contrast, and reduce image noise while preserving the edges of the particles. The particle size distribution is determined by measuring Dcirc = 2(area of projected image / 7t)1 / 2on at least 50000, typically 50,000 to 200,000 particles, at each magnification.
[0089] The pellets according to the various embodiments herein may be combined with EPDM and one or more optional additional elastomers to form elastomer composites. The resulting elastomer composite may include 80-200 phr particulate filler, for example, 100-190 or 120-180 or 140 to 175 or 150 to 170 phr particulate filler. Exemplary additional elastomers include polyolefin elastomer (POE), nitrile butadiene rubber (NBR), and hydrogenated nitrile butadiene rubber (HNBR). Such additional rubbers may improve the processability or chemical resistance of the EPDM profiles. For example, the pellets may be combined with an elastomer to form a masterbatch, which is then combined with additional elastomer of the same or different composition. Alternatively or in addition, two or more elastomers may be blended prior to mixing with the pellets. Alternatively or in addition, the elastomer composite may also contain one or more fillers aside from reclaimed carbon, including any of the particulate fillers listed elsewhere herein and any other fillers known to those of skill in the art for use in elastomer composites. Such fillers may be in a mixture or pellet with the milled reclaimed carbon or may be added to the elastomer separately from any of the pellets according to the various embodiments herein.
[0090] The elastomer composite may further comprise additives to facilitate mixing, promote vulcanization, or confer particular properties on a vulcanizate of the elastomer composite. Numerous additives are well known to those skilled in the art and include, for example, adhesion promoters, antioxidants, antiozonants, coupling agents, curatives, degradation inhibitors, plasticizers, processing aids (e.g., liquid polymers, oils and the like), oil extenders, wax, resins, flame-retardants, extender oils, lubricants, tackifiers, vulcanization activators such as zinc oxide and fatty acids, vulcanization accelerators, and a mixture of any of them. Exemplary additives include but are not limited to zinc oxide and stearic acid. The general use and selection of such additives is well known to those skilled in the art.
[0091] Dried pellets may be combined with elastomer as described above using any dry mixing method known to those of skill in the art.
[0092] Alternatively or in addition, wet pellets may be combined with elastomer according to the teachings of one or more of US20220332016, WO2021247153, WO2022125679, WO2022125683, WO2022125677, and WO2022125675, the entire contents of all of which are incorporated herein by reference. For example, the wet pellets and elastomer in solid form may be charged into a mixer and mixed under conditions where temperatures are controlled to remove at least a portion of the water in the pellets via evaporation. The elastomer is optionally premasticated prior to introduction of the wet pellets. The wet filler may be added all at once or in aliquots.
[0093] Any suitable mixer, such as a Banbury or Brabender mixer or other internal or closed mixer, or an open mixer, or an extruder or a continuous compounder or a kneading mixer or a combination thereof, may be employed to combine wet pellets with elastomer. Other mixers include a kneading type internal mixer. Commercially available internal mixers from Farrel- Pomini, Harburg Freudenberger Maschinenbau GmbH (HF), Kobelco, or Pelmar Eng'r Ltd can be used. Besides the option to use inner circuits of steam or water or other fluid in the rotors, in addition or alternatively, the internal mixer can have cooling or heating jackets at one region or part or more than one region or part of the mixing chamber to control the temperature of the components being mixed therein. This can create one or more heating / cooling zones in a wall or portion of a wall of a mixer. The mixer can be a single stage mixer or a multi-stage mixer (e.g., two stages or more). Examples of mixers and designs that can be utilized are described in European Patent No. 2423253B1 and U.S. Pat. No. 7,556,419, the disclosures of which are incorporated herein by reference.
[0094] As another option, the mixer can be a continuous mixer. For example, the solid elastomer and wet filler may be mechanically worked by using one or more of a continuous internal mixer, a twin screw extruder, a single screw extruder, or a roll mill, such as those described in U.S. Pat. No. 9,855,686 B2, the disclosure of which is incorporated herein by reference. Suitable kneading and masticating devices are well known and commercially available, including for example, a Unimix Continuous Mixer and MVX (Mixing, Venting, eXtruding) Machine from Farrel Pomini Corporation of Ansonia, Conn., an FCM™ Farrel Continuous Mixer, a long continuous mixer from Pomini, Inc., a Pomini Continuous Mixer, twin rotor corotating intermeshing extruders, twin rotor counterrotating non-intermeshing extruders, continuous compounding extruders, the biaxial milling extruder produced by Kobe Steel, Ltd., and a Kobe Continuous Mixer. Alternative masticating apparatus suitable for use with one or more embodiments disclosed herein will be familiar to those of skill in the art.
[0095] The mixing can be performed with a mixer(s) having at least one rotor and the mixer can be one or more of the following: a kneader, a roll mill, a screw extruder, a twin-screw extruder, a multiple-screw extruder, a continuous compounder, and / or a twin-screw extruder. The mixing can be performed with a mixer(s) having at least one rotor and the mixer can have two-wing rotors, four-wing rotors, six-wing rotors, eight-wing rotors, and / or one or more screw rotors.
[0096] The mixing process to combine wet pellets with elastomer may be a one stage (single stage) or multi-stage (multi-step) process. In a multi-stage process, one or more mixers or mixer types may be employed. For stages where an internal mixer is used, the fill factor at each such stagemay independently be no more than 72%, no more than 70%, or no more than 68%, or no more than 66%, such as from about 30% to 72%, from 40% to 70%, from 45% to 70%, from 30% to 60%, from 50 to 72%, from 50 to 70%, from 50 to 68%, from 60 to 72%, from 60 to 70%, from 60 to 68%, from 65 to 72%, from 65 to 70%, from 65 to 68%, or from 40 to 60% or from 50 to 60% and the like. The temperature of the mixer may be controlled to control the temperature of the mixture, the amount of water evaporated, or both. For example, in a multi-stage process, the temperature of the mixer for each stage may be controlled to control the amount of water evaporated from the mixture in the first mixing stage and in one or more subsequent stages. For instance, the liquid content of the composite discharged can be lower than the liquid content of the material charged into the mixer by an amount of from 10% to 99.9% (wt. % vs wt. %), from 10% to 95%, or from 10% to 50%. Alternatively or in addition, the rate of rate of liquid release from the composite or mixture during mixing, e.g., by evaporation, can be measured as a time average release rate of the liquid per kg of composite or mixture (e.g., total liquid removed / (release time x composite weight), and this rate can be from 0.01 to 0.14 kg / (min kg) or from 0.01 to 0.07 kg / (min kg) or other rates below or above this range.
[0097] Alternatively or in addition, the mixing process to combine wet pellets with elastomer may be controlled in one or more stages to allow a predetermined total specific energy (energy applied to a mixing system that drives one or more rotors per mass of composite on a dry weight basis), e g. from 1000 kJ / kg composite (or per kg mixture present in the mixer) to 10,000 kJ / kg composite (or per kg mixture present in the mixer), for example from 2,000 kJ / kg to 5,000 kJ or 1,500 kJ / kg to 8,000 kJ / kg, 1,500 kJ / kg to 7,000 kJ / kg, 1,500 kJ / kg to 6,000 kJ / kg, 1,500 kJ / kg to 5,000 kJ / kg, 1,500 kJ / kg to 3,000 kJ / kg, 1,600 kJ / kg to 8,000 kJ / kg, 1,600 kJ / kg to 7,000 kJ / kg, 1,600 kJ / kg to 6,000 kJ / kg, 1,600 kJ / kg to 5,000 kJ / kg, 1,600 kJ / kg to 4,000 kJ / kg, 1,600 kJ / kg to 3,000 kJ / kg, or other values in any of these ranges. Alternatively or in addition, the specific energy applied to the mixture may be divided to ensure a certain amount of specific energy is applied before or after a portion, e.g., 75% of the filler, is added to the mixer. That is, the filler need not be added all at once. Mixing times at each stage may be any suitable time, for example, from 1 min to 40 min, from 1 min to 20 min, from 1 min to 15 min, from 5 min to 30 min, from 5 min to 20 min , from 5 min to 15 min, or from 1 min to 12 min, from 1 min to 10 min, from 3 min to 30 min. or other times. Alternatively or in addition, the dump discharge temperature for each stage may be from 120° C. to 180° C., 120° C. to 190° C., 130° C. to 180° C., such as from 140° C. to 180° C., from 150° C. to 180° C , from 130° C. to 170° C., from 140° C. to 170° C., from 150° C. to 170° C , or other temperatures within or outside of these ranges.
[0098] Following any one or more mixing steps or stages, the resulting composite may be subjected to one or more post-processing steps, for example, to shape or form the composite and / or allow for improved handling. Post-processing may provide a composite that can be dried, homogenized, extruded, calendared, milled, granulated, cut, baled, or sheeted. The composite may be compounded and vulcanized immediately or may be held for a period of time prior to compounding. Suitable equipment for various post-processing steps includes but are not limited to one or more of an internal mixer, a kneader, a roll mill, an open mill, a screw extruder, a twin- screw extruder, a multiple-screw extruder, a continuous compounder, and / or a twin screw discharge extruder fitted with a roller die (e.g., twin-screw sheeter) or fitted with stationary knives. Depending on which device or devices are used, it may be desirable to process the composite through the device more than one time or through a series of like or different devices having the same or different operating settings (e.g., speed, temperature, energy input, etc.). Alternatively or in addition, the elastomer composite may be combined with added filler, added elastomer, or both, prior to or as part of the vulcanization process. The additional filler may be the same or different as the particulate filler in the elastomer composite and may include any filler known to those of skill in the art, including the fillers listed as additional and supplemental fillers in this case and including additional wet milled reclaimed carbon. The added filler and or elastomer may increase or decrease the filler loading of the vulcanizate with respect to the elastomer composite.
[0099] To vulcanize elastomer composite material, it is combined with a curative package including a cross-linking agent, any necessary activators and accelerators, anti-oxidant, and additional optional additives such as any of those listed above. Where sulfur is used as a crosslinking agent, typical activators include zinc oxide and or stearic acid, and typical accelerators include thiazole such as 2-2’-dithiobis (benzothiazole) (MBTS), sulfenamides such as N- cyclohexyl-2-benzothiazole sulfonamide (CBS), dithiocarbamate such as zinc dibenzyldithiocarbamte (ZDBC). Anti-oxidants include N-(l,3-dimethylbutyl)-N’-phenyl-p- phenylenediamine (6PPD) and those listed in WO2012 / 037244. Other curatives used in rubber processing are peroxides, urethane crosslinkers, metallic oxides, acetoxysilane compounds, and so forth. Additional suitable components for sulfur-based and other cross-linking systems and methods of mixing and vulcanizing elastomer composites are well known to those of skill in the art. For example, typical procedures used for rubber compounding are described in Maurice Morton, Rubber Technology, 3rd Edition, Van Norstrand Reinhold Company, New York 1987, and 2nd Edition, Van Nordstrand Reinhold Company, New York 1973.
[0100] A variety of rubber articles may incorporate the vulcanizate. Preferably, the rubber product, as indicated, is an EPDM product or profile, such as EPDM weather stripping and the like. The rubber article or product can be in the form of or shape of a hose, membrane, and similar types of articles and products. Essentially, any rubber article where surface defects are important or critical to performance and / or appearance, the present invention can be utilized.
[0101] The present invention includes the following aspects / embodiments / features in any order and / or in any combination:
[0102] 1 An EPDM profile extruded from an EPDM formulation comprising a mixture of80-200 phr of solid pellets and at least one EPDM polymer having either a thermodynamic transition at a temperature less than 30°C or an ethylene content less than 60 wt%, and wherein said solid pellets comprise a milled blend of reclaimed carbon and virgin carbon black, and wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 250 or less, b) Surface Defect size 100 to 125 microns — a surface defect count of 200 or less, c) Surface Defect size 125 to 150 microns — a surface defect count of 100 or less, d) Surface Defect size 150 to 200 microns — a surface defect count of 150 or less, e) Surface Defect size 200 to 250 microns — a surface defect count of 50 or less, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 35 or less, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
[0103] 2. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 100 to 250 or 100 to 230, b) Surface Defect size 100 to 125 microns — a surface defect count of 100 to 200 or 100 to 150, c) Surface Defect size 125 to 150 microns — a surface defect count of 25 to 100 or 25 to 80, d) Surface Defect size 150 to 200 microns — a surface defect count of 50 to 150 or from 50 to 125, e) Surface Defect size 200 to 250 microns — a surface defect count of 10 to 50 or 10 to 25, and / orf) Surface Defect size greater than 250 microns — a surface defect count of 5 to 35 or 5 to 25, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
[0104] 3. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least two of a)-f) is present.
[0105] 4. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least three of a)-f) is present.
[0106] 5. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least four of a)-f) is present.
[0107] 6. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least five of a)-f) is present.
[0108] 7. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein all of a)-f) is present.
[0109] 8 An EPDM profile extruded from an EPDM formulation comprising a mixture of80-200 phr of solid pellets and at least one EPDM polymer having a thermodynamic transition at a temperature of at least 30°C and an ethylene content of at least 60 wt% , and wherein said solid pellets comprise a milled blend of reclaimed carbon and virgin carbon black, and wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 120 or less, b) Surface Defect size 100 to 125 microns — a surface defect count of 70 or less, c) Surface Defect size 125 to 150 microns — a surface defect count of 25 or less, d) Surface Defect size 150 to 200 microns — a surface defect count of 25 or less, e) Surface Defect size 200 to 250 microns — a surface defect count of 8 or less, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 11 or less, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
[0110] 9 The EPDM profile of any preceding or following embodiment / feature / aspect, wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 50 to 120 or 50 to 90, b) Surface Defect size 100 to 125 microns — a surface defect count of 25-70 or 25 to 40, c) Surface Defect size 125 to 150 microns — a surface defect count of 5 to 25 or 5 to 20, d) Surface Defect size 150 to 200 microns — a surface defect count of 13 to 25 or 13-22,e) Surface Defect size 200 to 250 microns — a surface defect count of 3 to 8 or 3 to 6, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 3 to 11 or 3 to 10, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
[0111] 10. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least two of a)-f) is present.
[0112] 11. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least three of a)-f) is present.
[0113] 12. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least four of a)-f) is present.
[0114] 13. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein at least five of a)-f) is present.
[0115] 14. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein all of a)-f) is present.
[0116] 15. The EPDM profile of any preceding or following embodiment / feature / aspect, wherein EPDM profile comprises 100-190 phr of the milled blend, for example, 120-180 phr, 140 to 175 phr, or 150 to 170 phr.
[0117] 16. A method of making the EPDM profile of any preceding or following embodiment / feature / aspect, said method comprising blending the at least one EPDM polymer with a plurality of the solid pellets to form the EPDM formulation, and extruding the EPDM formulation to form the EPDM profile.
[0118] 17. A method of making a solid pellet, said method comprising feeding reclaimed carbon and feeding virgin carbon black as separate feeds to a mill; milling the reclaimed carbon and the virgin carbon black together to obtain a milled blend; wet pelletizing the milled blend to obtain wet solid pellets; drying the wet solid pellets to obtain dry solid pellets.
[0119] 18. The method of any preceding or following embodiment / feature / aspect, wherein the milling comprises hammer milling.
[0120] 19. The method of any preceding or following embodiment / feature / aspect, wherein the milling is dry milling.
[0121] 20. The method of any preceding or following embodiment / feature / aspect, wherein the milling comprises pin milling, air classification milling, long gap milling, jet milling, or media milling.
[0122] 21. The method of any preceding or following embodiment / feature / aspect, wherein the virgin carbon black is fed directly from a carbon black production line.
[0123] 22. The method of any preceding or following embodiment / feature / aspect, wherein the virgin carbon black has a temperature of from 100 deg C to 200 deg C.
[0124] 23. The method of any preceding or following embodiment / feature / aspect, wherein the virgin carbon black is ASTM 300 to 500 series.
[0125] 24. The method of any preceding or following embodiment / feature / aspect, wherein said wet pelletizing comprises blending the milled blend with an aqueous solution and at least one binder and then forming said wet solid pellets.
[0126] 25. The method of any preceding or following embodiment / feature / aspect, wherein the amount of the at least one binder is from 100 ppm to 4000 ppm.
[0127] 26. The method of any preceding or following embodiment / feature / aspect, wherein said milling is sufficient to obtain a milled blend having a D90 in a range of from 0.3 micron to 1.0 micron for the virgin carbon black and a D90 in a range of from <10 microns to <20 microns for the reclaimed carbon.
[0128] 27. The method of any preceding or following embodiment / feature / aspect, wherein the reclaimed carbon is fed to said mill in the absence of a pre-grinding or pre-milling.
[0129] 28. The method of any preceding or following embodiment / feature / aspect, wherein the reclaimed carbon has a D50 of 0.5 mm to 1 mm.
[0130] 29. A solid pellet comprising a blend of reclaimed carbon particles and virgin carbon black, wherein said virgin carbon black particles having a D90 in a range of from 0.3 micron to 1.0 micron for the virgin carbon black and a D90 in a range of from <10 microns to <20 microns for the reclaimed carbon.
[0131] 30. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the solid pellet further comprises at least one binder.
[0132] 31. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the binder is present in an amount of from 100 ppm to 4000 ppm.
[0133] 32. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the solid pellet has an average size of from about 0.5 mm to about 2 mm.
[0134] 33. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the solid pellet has a moisture content of less than 2 wt%.
[0135] 34. The solid pellet of any preceding or following embodiment / feature / aspect, wherein said reclaimed carbon particles are present in an amount of from 1 wt% to 50 wt%, and said virgin carbon black particles are present in an amount of from 50 wt% to 99 wt%, based on total weight of said solid pellet.
[0136] 35. The solid pellet of any preceding or following embodiment / feature / aspect, wherein said reclaimed carbon particles are present in an amount of from 5 wt% to 20 wt%, and said virgin carbon black particles are present in an amount of from 80 wt% to 95 wt%, based on total weight of said solid pellet.
[0137] 36. The solid pellet of any preceding or following embodiment / feature / aspect, wherein said reclaimed carbon particles are present in an amount of from 5 wt% to 15 wt%, and said virgin carbon black particles are present in an amount of from 85 wt% to 95 wt%, based on total weight of said solid pellet.
[0138] 37. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the solid pellet has a pellet hardness of from 30 grams to 45 grams , measured by ASTM D5230.
[0139] 38. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the virgin carbon black is an ASTM 300 to 500 series black.
[0140] 39. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the solid pellet has the property to provide an EPDM profile extruded from a formulation comprising a mixture of 80-200 phr of the solid pellets and at least one EPDM polymer having either a thermodynamic transition at a temperature less than 30°C or an ethylene content less than 60 wt%, one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 100 to 250 or 100 to 230, b) Surface Defect size 100 to 125 microns — a surface defect count of 100 to 200 or 100 to 150, c) Surface Defect size 125 to 150 microns — a surface defect count of 25 to 100 or 25 to 80, d) Surface Defect size 150 to 200 microns — a surface defect count of 50 to 150 or from 50 to 125, e) Surface Defect size 200 to 250 microns — a surface defect count of 10 to 50 or 10 to 25, and / orf) Surface Defect size greater than 250 microns — a surface defect count of 5 to 35 or 5 to 25, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
[0141] 40. The solid pellet of any preceding or following embodiment / feature / aspect, wherein the solid pellet has the property to provide an EPDM profile extruded from a formulation comprising a plurality of the solid pellets and at least one EPDM polymer having a thermodynamic transition at a temperature of at least 30oC and an ethylene content of at least 60 wt%, one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 50 to 120 or 50 to 90, b) Surface Defect size 100 to 125 microns — a surface defect count of 25-70 or 25 to 40, c) Surface Defect size 125 to 150 microns — a surface defect count of 5 to 25 or 5 to 20, d) Surface Defect size 150 to 200 microns — a surface defect count of 13 to 25 or 13-22, e) Surface Defect size 200 to 250 microns — a surface defect count of 3 to 8 or 3 to 6, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 3 to 11 or 3 to 10, wherein the surface defect count is based on a 165 cm2 section of the EPDM profile that is a tape and analyzed to determine the surface defect count.41. An EPDM profile extruded from an EPDM formulation comprising a mixture of 80- 200 phr of the solid pellets of any preceding or following embodiment / feature / aspect, and at least one EPDM polymer.
[0142] The present invention will be further clarified by the following examples which are intended to be only exemplary in nature.EXAMPLES
[0143] Example 1Three EPDM compounds were prepared with an amorphous polymer, Keltan 10660C EPDM (produced by Arlanxeo), and extruded into 1 mm thick tape. The formulations are shown in Table 1. All compositions were mixed in a 1.6 L Banbury mixer with two wing rotors. Dry mixed samples (pellet moisture <1 wt%) were prepared in two stages as described in Table 2. After each compounding stage, the compounds were sheeted on a 2-roll mill operated at 50°C and 20 rpm, followed by banding for 60 seconds and six pass-throughs with a nip gap about 3mm, with a rest time before next stage of mixing (or curing, after the last stage) of at least 3 hours. Curing wasperformed in a heated press (160°C, 2500 lbs), for a time T90 + 2min as determined by a conventional rubber rheometer, where T90 is the time to achieve 90% vulcanization. The rubber compounds were extruded with the Brabender extruder and a tape die. The barrel temperature was 100 °C, and the rotor speed was 30 rpm. The length, width, and thickness of a tape are about 25 cm, 2 cm, and 1 mm, respectively. The Inventive Example 1 (IE1) used co-pellets that included N550 carbon black from Cabot Corporation along with reclaimed carbon (rC) hammermilled to 500 mesh (10 wt% rC with 90 wt% virgin carbon black) that were wet pelletized with about 0.2 wt% sodium lignosulfonate as a 65 wt% slurry in a conventional pelletizer with walls maintained at about 86 deg C and then dried. The Comparative Example 1 (CE1) used N550 carbon black, while Comparative Example (CE2) used direct blends of 10 wt% of rC and 90 wt% of N550 CB (not co-pellets). All compounds were made with two replicates, and the results here are the average values of two replicates.Table 1: Formulation of EPDM weatherstrip compoundsIn Table 1, CaCO3 is produced by NuoboSunpar 2280 is parrafinic oil produced by Sun Oil CompanyStearic acid is produced by IOI OleochemicalsZnO-80 is provided by ActmixPEG4000 is provided by Lotte ChemicalCaO-80 is desiccant, produced by ActmixCBS-80 is 80% N-Cyclohexyl-2-benzothiazole sulfenamide, 20 % elastomer binder and dispersing agents, produced by Rhein ChemieRetarder E-80GE is 80 % sulfonamide derivative 20 % elastomer binder and dispersing agents, produced by Rhein Chemie.MBTS-75 is 75% 2-2’-Dithiobis(benzothiazole), 25 % elastomer binder and dispersing agents produced by Rhein Chemie.CLD-80 is 80% caprolactam disulfide, 20 % elastomer binder and dispersing agents produced by Rhein Chemie.TP-50 is 50% zinc dialkyldithiophosphate, 50 % elastomer binder and dispersing agents produced by Rhein Chemie.ZBEC-70 is 70 % zinc-dibenzyl-dithiocarbamate, 30 % elastomer binder and dispersing agents produced by Rhein Chemie.S-80 is 80% Sulfur, 20% elastomer binder and dispersing agents produced by Rhein Chemie.
[0144] TABLE 2:
[0145] The surfaces of extruded EPDM tapes were measured via an optical video system from Suzhou Oi-Smart Technology Co. to analyze the surface defects. The pictures of the tape surface are shown in FIG. 1. The black areas on the surface are the defects. The pictures show the same trend as observed by naked eye that IE1 (rC and carbon black co-pellet) resulted in significantly less surface defects than CE2 (direct blends of rC and N550 carbon black). Moreover, the IE1 had a visual appearance similar to CE1 (N550 carbon only). The statistical analysis of the surface defects of 165 cm2extruded tapes is provided in FIG. 2. The defect counts of IE1 are slightly higher or comparable to those of CE1. The defect counts of IE1 are 50-70% lower than those of CE2 for all size ranges, showing that the rC-CB co-pellet did effectively reduce the quantity of surface defects compared to direct blends. The surface defects of the extruded profiles were measured by an automatic visual inspection machine. The camera scans the surface of the profile and automatically recognizes and measures the defects as areas of contrast with the background with a line speed of lOmm / s, a measuring field width of 28 mm, and a pixel resolution of 7 microns. The scanned surface area for each profile is 165 cm2.
[0146] The volume resistivity (EVR) of the three examples were also tested and the results are shown in FIG. 3. The EVR follows the order that IE1 > CE2 > CE1. rC usually has higher EVR than regular carbon black due to its morphology, surface functionality, and possibly ash residue. The higher EVR of IE1 than CE2 indicates that rC is dispersed better in IE1 than CE2, which serves as “a more electrically resistive layer” within the CB network and increases the volume resistivity. The EVR results can support the belief that co-pelletization improves the dispersion of rC.
[0147] The mechanical properties were also tested for the three samples and the results are set forth in Table 3.
[0148] Table 3
[0149] Example 2
[0150] Three EPDM compounds using a semicrystalline EPDM, Nordel 4785HM polymer (produced by Dow), were prepared and extruded into 1 mm thick tape. The formulations are shown in Table 4. All compositions were mixed in a 1.6 L Banbury mixer with two wing rotors. Dry mixed samples (pellet moisture <1 wt%) were prepared in two stages as described in Table 5. After each compounding stage, the compounds were sheeted on a 2-roll mill operated at 50°C and about 20 rpm, followed by banding for 60 seconds and six pass-throughs with a nip gap about 3 mm, with a rest time before next stage of mixing (or curing, after the last stage) of at least 3 hours. Curing was performed in a heated press (160 °C, 2500 lbs), for a time T90 + 2min as determined by a conventional rubber rheometer, where T90 is the time to achieve 90% vulcanization. The rubber compounds were extruded with the Brabender extruder and a tape die. The barrel temperature was 100 °C, and the rotor speed was 30 rpm. The length, width, and thickness of a tape are about 25 cm, 2 cm, and 1 mm, respectively. The Inventive Example 2 (IE2) used co-pellets that included N55O carbon black from Cabot Corporation along with reclaimed carbon (rC) hammermilled to 500 mesh (10 wt% rC with 90 wt% virgin carbon black). The Comparative Example 1 (CE3) used N550 carbon black, while Comparative Example (CE4) used direct blends of 10 wt% of rC and 90 wt% of N550 CB (not co-pellets).Table 4: Formulation of EPDM weatherstrip compoundsIn Table 4, ZDTP-50 is zinc alkyl dithiophosphate, 50 % elastomer binder and dispersing agents produced by Rhein Chemie; all other components are as listed in Table 1.
[0151] TABLE 5:
[0152] The surfaces of extruded EPDM tapes were measured via an optical video system to analyze the surface defects as described in Example 1. The statistical analysis of the surface defects of 165 cm2extruded tapes is provided in FIG. 5 and show that the use of N550-rC copellets resulted in the lowest number of defects, lower even than with the use of neat carbon black.Themechanical properties were also tested for the three samples and the results are set forth in Table 6.
[0153] Table 6
[0154] Example 3
[0155] Two EPDM compounds using a semicrystalline EPDM, Nordel 4785HM polymer (produced by Dow), are prepared and extruded into 1 mm thick tape. The formulations are shown in Table 7. All compositions are mixed in a 1.6 L Banbury mixer with two wing rotors. Dry mixed samples (pellet moisture <1 wt%) were prepared in two stages as described in Table 8. After each compounding stage, the compounds are sheeted on a 2-roll mill operated at 50°C and about 20 rpm, followed by banding for 60 seconds and six pass-throughs with a nip gap about 3 mm, with a rest time before next stage of mixing (or curing, after the last stage) of at least 3 hours. Curing is performed in a heated press (160 °C, 2500 lbs), for a time T90 + 2min as determined by a conventional rubber rheometer, where T90 is the time to achieve 90% vulcanization. The rubber compounds is extmded with the Brabender extruder and a tape die. The barrel temperature is 100 °C, and the rotor speed is 30 rpm. The length, width, and thickness of a tape are about 25 cm, 2 cm, and 1 mm, respectively. The compounds use co-pellets produced as in Example 1. It is expected that such compounds will exhibit a lower level of surface defects than with the use of blends of N550 carbon black pellets and rC pellets.TABLE 7In Table 7, ZDTP-50 is zinc alkyl dithiophosphate, 50 % elastomer binder and dispersing agents produced by Rhein Chemie; all other components are as listed in Table 1.TABLE 8:
[0156] While this invention has been particularly shown and described with references to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention encompassed by the appended claims.
[0157] As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items. Also, all conjunctions used are to be understood in the most inclusive sense possible. Thus, the word "or" should be understood as having the definition of a logical "or" rather than that of a logical "exclusive or" unless the context clearly necessitates otherwise. Further, the singular forms and the articles "a", "an" and "the" are intended to include the plural forms as well, unless expressly stated otherwise. It will be further understood that the terms: includes, comprises, including and / or comprising, when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof. Further, it will be understood that when an element, including component or subsystem, is referred to and / or shown as being connected or coupled to another element, it can be directly connected or coupled to the other element or intervening elements may be present.
[0158] It will be understood that although terms such as “first” and “second” are used herein to describe various elements, these elements should not be limited by these terms. These terms are only used to distinguish one element from another element. Thus, an element discussed below could be termed a second element, and similarly, a second element may be termed a first element without departing from the teachings of the present invention.
[0159] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
[0160] Applicants specifically incorporate the entire contents of all cited references in this disclosure. Further, when an amount, concentration, or other value or parameter is given as either a range, preferred range, or a list of upper preferable values and lower preferable values, this is tobe understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. Where a range of numerical values is recited herein, unless otherwise stated, the range is intended to include the endpoints thereof, and all integers and fractions within the range. It is not intended that the scope of the invention be limited to the specific values recited when defining a range. It is further understood that for any range provided herein, the numerical ranges can be “about” these ranges, and vice versa, where a range is provided using “about” ranges, these ranges can be precisely the number ranges provided. Any combination of embodiments, and / or ingredients and / or components and / or properties recited herein can be made herein and is considered part of the present invention
[0161] Other embodiments of the present invention will be apparent to those skilled in the art from consideration of the present specification and practice of the present invention disclosed herein. It is intended that the present specification and examples be considered as exemplary only with a true scope and spirit of the invention being indicated by the following claims and equivalents thereof.
Claims
CLAIMS1. An EPDM profile extruded from an EPDM formulation comprising a mixture of 80-200 phr of solid pellets and at least one EPDM polymer having either a thermodynamic transition at a temperature less than 30°C or an ethylene content less than 60 wt%, and wherein said solid pellets comprise a milled blend of reclaimed carbon and virgin carbon black, and wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 250 or less, b) Surface Defect size 100 to 125 microns — a surface defect count of 200 or less, c) Surface Defect size 125 to 150 microns — a surface defect count of 100 or less, d) Surface Defect size 150 to 200 microns — a surface defect count of 150 or less, e) Surface Defect size 200 to 250 microns — a surface defect count of 50 or less, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 35 or less, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
2. The EPDM profile of claim 1 , wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 100 to 250 or 100 to 230, b) Surface Defect size 100 to 125 microns — a surface defect count of 100 to 200 or 100 to 150, c) Surface Defect size 125 to 150 microns — a surface defect count of 25 to 100 or 25 to 80, d) Surface Defect size 150 to 200 microns — a surface defect count of 50 to 150 or from 50 to 125, e) Surface Defect size 200 to 250 microns — a surface defect count of 10 to 50 or 10 to 25, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 5 to 35 or 5 to 25, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
3. The EPDM profile of claim 1 or 2, wherein at least two of a)-f) is present.
4. The EPDM profile of claim 1 or 2, wherein at least three of a)-f) is present.
5. The EPDM profile of claim 1 or 2, wherein at least four of a)-f) is present.
6. The EPDM profile of claim 1 or 2, wherein at least five of a)-f) is present.
7. The EPDM profile of claim 1 or 2, wherein all of a)-f) is present.
8. An EPDM profile extruded from an EPDM formulation comprising a mixture of 80-200 phr of solid pellets and at least one EPDM polymer having a thermodynamic transition at a temperature of at least 30°C and an ethylene content of at least 60 wt% , and wherein said solid pellets comprise a milled blend of reclaimed carbon and virgin carbon black, and wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 120 or less, b) Surface Defect size 100 to 125 microns — a surface defect count of 70 or less, c) Surface Defect size 125 to 150 microns — a surface defect count of 25 or less, d) Surface Defect size 150 to 200 microns — a surface defect count of 25 or less, e) Surface Defect size 200 to 250 microns — a surface defect count of 8 or less, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 11 or less, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
9. The EPDM profile of claim 8, wherein the EPDM profile has one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 50 to 120 or 50 to 90, b) Surface Defect size 100 to 125 microns — a surface defect count of 25-70 or 25 to 40, c) Surface Defect size 125 to 150 microns — a surface defect count of 5 to 25 or 5 to 20, d) Surface Defect size 150 to 200 microns — a surface defect count of 13 to 25 or 13- 22, e) Surface Defect size 200 to 250 microns — a surface defect count of 3 to 8 or 3 to 6, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 3 to 11 or 3 to 10, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
10. The EPDM profile of claim 8 or 9, wherein at least two of a)-f) is present.
11. The EPDM profile of claim 8 or 9, wherein at least three of a)-f) is present.
12. The EPDM profile of claim 8 or 9, wherein at least four of a)-f) is present.
13. The EPDM profile of claim 8 or 9, wherein at least five of a)-f) is present.
14. The EPDM profile of claim 8 or 9, wherein all of a)-f) is present.
15. The EPDM profile of any of the preceding claims, wherein EPDM profile comprises 100-190 phr of the milled blend, for example, 120-180 phr, 140 to 175 phr, or 150 to 170 phr.
16. A method of making the EPDM profile of any preceding claim, said method comprising blending the at least one EPDM polymer with a plurality of the solid pellets to form the EPDM formulation, and extruding the EPDM formulation to form the EPDM profile.
17. A method of making a solid pellet, said method comprising feeding reclaimed carbon and feeding virgin carbon black as separate feeds to a mill; milling the reclaimed carbon and the virgin carbon black together to obtain a milled blend; wet pelletizing the milled blend to obtain wet solid pellets; drying the wet solid pellets to obtain dry solid pellets.
18. The method of claim 17, wherein the milling comprises hammer milling.
19. The method of claim 17, wherein the milling is dry milling.
20. The method of claim 17, wherein the milling comprises pin milling, air classification milling, long gap milling, jet milling, or media milling.
21. The method of any of claims 17-20, wherein the virgin carbon black is fed directly from a carbon black production line.
22. The method of any of claims 17-21, wherein the virgin carbon black has a temperature of from 100 deg C to 200 deg C.
23. The method of any of claims 17-22, wherein the virgin carbon black is ASTM 300 to 500 series.
24. The method of any of claims 17-23, wherein said wet pelletizing comprises blending the milled blend with an aqueous solution and at least one binder and then forming said wet solid pellets.
25. The method of any of claims 17-24, wherein the amount of the at least one binder is from 100 ppm to 4000 ppm.
26. The method of any of claims 17-25, wherein said milling is sufficient to obtain a milled blend having a D90 in a range of from 0.3 micron to 1.0 micron for the virgin carbon black and a D90 in a range of from <10 microns to <20 microns for the reclaimed carbon.
27. The method of any of claims 17-26, wherein the reclaimed carbon is fed to said mill in the absence of a pre-grinding or pre-milling.
28. The method of claims 17-27, wherein the reclaimed carbon has a D50 of 0.5 mm to 1 mm.
29. A solid pellet comprising a blend of reclaimed carbon particles and virgin carbon black, wherein said virgin carbon black particles having a D90 in a range of from 0.3 micron to 1.0 micron for the virgin carbon black and a D90 in a range of from <10 microns to <20 microns for the reclaimed carbon.
30. The solid pellet of claim 29, wherein the solid pellet further comprises at least one binder.
31. The solid pellet of claim 29 or 30, wherein the binder is present in an amount of from 100 ppm to 4000 ppm.
32. The solid pellet of any of claims 29-31, wherein the solid pellet has an average size of from about 0.5 mm to about 2 mm.
33. The solid pellet of any of claims 29-32, wherein the solid pellet has a moisture content of less than 2 wt%.
34. The solid pellet of any of claims 29-33, wherein said reclaimed carbon particles are present in an amount of from 1 wt% to 50 wt%, and said virgin carbon black particles are present in an amount of from 50 wt% to 99 wt%, based on total weight of said solid pellet.
35. The solid pellet of any of claims 29-34, wherein said reclaimed carbon particles are present in an amount of from 5 wt% to 20 wt%, and said virgin carbon black particles are present in an amount of from 80 wt% to 95 wt%, based on total weight of said solid pellet.
36. The solid pellet of any of claims 29-35, wherein said reclaimed carbon particles are present in an amount of from 5 wt% to 15 wt%, and said virgin carbon black particles are present in an amount of from 85 wt% to 95 wt%, based on total weight of said solid pellet.
37. The solid pellet of any of claims 29-36, wherein the solid pellet has a pellet hardness of from 30 grams to 45 grams , measured by ASTM D5230.
38. The solid pellet of any of claims 29-37, wherein the virgin carbon black is an ASTM 300 to 500 series black.
39. The solid pellet of any of claims 29-38, wherein the solid pellet has the property to provide an EPDM profile extruded from a formulation comprising a mixture of 80-200 phr of the solid pellets and at least one EPDM polymer having either a thermodynamic transition at a temperature less than 30°C or an ethylene content less than 60 wt%, one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 100 to 250 or 100 to 230, b) Surface Defect size 100 to 125 microns — a surface defect count of 100 to 200 or 100 to 150, c) Surface Defect size 125 to 150 microns — a surface defect count of 25 to 100 or 25 to 80, d) Surface Defect size 150 to 200 microns — a surface defect count of 50 to 150 or from 50 to 125, e) Surface Defect size 200 to 250 microns — a surface defect count of 10 to 50 or 10 to 25, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 5 to 35 or 5 to 25, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
40. The solid pellet of any of claims 29-39, wherein the solid pellet has the property to provide an EPDM profile extruded from a formulation comprising a plurality of the solid pellets and at least one EPDM polymer having a thermodynamic transition at a temperature of at least 30°C and an ethylene content of at least 60 wt%, one or more of the following surface defect counts: a) Surface Defect size 80 to 100 microns — a surface defect count of 50 to 120 or 50 to 90, b) Surface Defect size 100 to 125 microns — a surface defect count of 25-70 or 25 to 40, c) Surface Defect size 125 to 150 microns — a surface defect count of 5 to 25 or 5 to 20, d) Surface Defect size 150 to 200 microns — a surface defect count of 13 to 25 or 13- 22,e) Surface Defect size 200 to 250 microns — a surface defect count of 3 to 8 or 3 to 6, and / or f) Surface Defect size greater than 250 microns — a surface defect count of 3 to 11 or 3 to 10, wherein the surface defect count is based on a 165 cm2section of the EPDM profile that is a tape and analyzed to determine the surface defect count.
41. An EPDM profile extruded from an EPDM formulation comprising a mixture of 80-200 phr of the solid pellets of any one of claims 29-40, and at least one EPDM polymer.
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