Composite material and method for obtaining same

Abstract

The present disclosure provides a composite material comprising an intimate blend of: (a) at least about 40% w / w of a total composite weight of non-plastic organic material, the non-plastic organic material comprising at least cellulose; (b) about 5% w / w to about 60% w / w of a total composite weight of plastic material, the plastic material comprising a plurality of synthetic thermoplastic polymers; and (c) up to 15% w / w of an inorganic material, wherein the composite material comprises an aryl-containing synthetic polymer in an amount less than 10% of the total composite weight; and wherein the composite material is characterized by at least one of the following properties: (i) the composite material has a notched Izod impact of at least 15 h / m; and (ii) an injection-molded sample of the composite material has at least one of a tensile strength of at least 8 MPa and a flexural strength of at least 15 MPa. Also provided are methods for preparing composite materials that involve the use of a heterogeneous incorporation material that includes an aryl-containing synthetic polymer in an amount less than 10% of the total weight of the composite material, and methods for producing articles of manufacture from the composite materials.

Description

[Technical Field]

[0001] The present disclosure relates to waste management, and in particular to composite materials derived from waste materials.

[0002] References The following references are considered to be relevant as background to the subject matter disclosed herein. -International Patent Application Publication No. 2010 / 082202 -International Patent Application Publication No. 12007949 -U.S. Patent No. 6,692,544

[0003] Acknowledgment of the above references herein should not be inferred as meaning that they are in any way relevant to the patentability of the subject matter disclosed herein. [Background technology]

[0004] Only a small proportion of the municipal waste generated is actually recycled into useful products.

[0005] International Patent Application Publication No. 2010 / 082202 describes a composite material having thermoplastic properties and comprising an organic material and, optionally, one or both of an inorganic material and a plastic, which can be prepared from waste materials such as household waste. The composite material is processed to obtain a useful article. This composite material can be combined with a second component comprising at least one element selected from the group consisting of vulcanized rubber and tire cord, as described in International Patent Application Publication No. 12007949.

[0006] U.S. Patent No. 6,692,544 describes the formation of briquettes and pellets from different types of waste materials, including municipal solid waste, which are either used as fuel in waste-to-energy processes or disposed of in landfills. Summary of the Invention

[0007] The present disclosure is based on the development of a technology that allows for unexpected and significant improvements in the physical properties of composite materials produced from heterogeneous waste. Specifically, the technology is based on removing selected types of synthetic polymers, as defined below, from the heterogeneous waste prior to subjecting the waste to heating and mixing under shear. The technology thus provides superior composite materials, methods for obtaining same, and uses thereof.

[0008] Thus, according to a first of the aspects of the present disclosure, the present disclosure provides a composite material, the composite material comprising: a. at least about 40% w / w of a total weight of the composite material of non-plastic organic material, the non-plastic organic material comprising at least cellulose; b. about 5% w / w to about 60% w / w of a plastic material by total weight of the composite material, the plastic material comprising a plurality of synthetic thermoplastic polymers; c. A homogeneous blend of up to 15% w / w of inorganic materials, the composite material comprises an aryl-containing synthetic polymer in an amount less than 10% of the total weight of the composite material; The composite material has the following properties: - the composite has a notched Izod impact of at least 15 h / m, and - the composite material sample subjected to injection molding a tensile strength of at least 8 MPa, and and a flexural strength of at least 15 MP.

[0009] In some instances, the composite material is 1.2 gr / cm 3 It is characterized by the following densities:

[0010] In some examples, the composite is characterized by a notched Izod impact of at least 15 J / m.

[0011] In some examples, the composite material is characterized by a thermal gravimetry analysis (TGA) temperature greater than 200°C.

[0012] In some examples, when a sample of the composite material is subjected to injection molding, the injection molded sample is characterized by a tensile strength of at least 10 MPa.

[0013] In some examples, when a sample of the composite material is subjected to injection molding, the injection molded sample is characterized by a tensile modulus of at least 1,500 MPa.

[0014] In some examples, when a sample of the composite material is subjected to injection molding, the injection molded sample is characterized by a flexural modulus of at least 1,500 MPa.

[0015] In some instances, a sample of the composite material, when subjected to injection molding, has a flexural strength of at least 20 MPa; In some examples, the composite material comprises less than 5 mg / g of silicate.

[0016] The composite materials disclosed herein can be characterized by any combination of two or more of the above features, with each feature and each possible combination constituting a separate embodiment of the present disclosure.

[0017] As demonstrated by the non-limiting examples provided herein, the composite materials have exceptionally low amounts of aryl-containing synthetic polymers compared to the amounts in unsorted heterogeneous household waste.

[0018] Also disclosed herein are methods for preparing the composite materials disclosed herein.

[0019] In some embodiments, the method comprises subjecting the particulate heterogeneous incorporation material to at least one extrusion process at a temperature maintained within the range of 150°C and 200°C, thereby obtaining the composite material; The particulate foreign incorporation material is i. at least about 40% w / w of non-plastic organic matter by total weight of the heterogeneous waste, the non-plastic organic matter comprising at least cellulose; ii. about 5% w / w to about 60% w / w of a plastic material by total weight of the composite, the plastic material comprising a plurality of synthetic thermoplastic polymers; iii. up to 15% w / w of inorganic material by total weight of the composite material; The heterogeneous incorporation material comprises an aryl-containing synthetic polymer in an amount less than 10% of the total weight of the composite material.

[0020] In some embodiments, the method includes subjecting the particulate heterogeneous waste to at least one separation step including removing incompatible plastics, including at least an aryl-containing synthetic polymer, from the particulate heterogeneous waste based on near-infrared (NIR) absorbance to obtain a heterogeneous incorporated material, and subjecting the heterogeneous incorporated material to at least one extrusion process at a temperature maintained within the range of 150°C and 200°C, thereby obtaining a composite material.

[0021] In some instances, the incompatible plastics that are removed include one or more halogenated polymers.

[0022] Also disclosed herein are articles of manufacture comprising an intimate blend of the composite materials disclosed herein and at least one polyolefin.

[0023] Additionally, disclosed herein are methods of producing articles of manufacture, the methods comprising processing a composite material disclosed herein with at least one polyolefin, the processing comprising at least one of extrusion and molding, the processing providing an intimate blend of the composite material with the at least one polyolefin. The following describes various aspects of the present invention, although they overlap with other descriptions. However, the present invention is not limited to the following. [1] A composite material comprising: a. at least about 40% w / w of a total weight of the composite material of non-plastic organic material, the non-plastic organic material comprising at least cellulose; b. about 5% w / w to about 60% w / w of a plastic material of the total weight of the composite material, the plastic material comprising a plurality of synthetic thermoplastic polymers; c. A homogeneous blend of up to 15% w / w of inorganic materials, the composite material comprises an aryl-containing synthetic polymer in an amount less than 10% of the total weight of the composite material; The composite material has the following properties: - the composite material has a notched Izod impact of at least 15 h / m, and - the sample of said composite material subjected to injection molding a tensile strength of at least 8 MPa, and a flexural strength of at least 15 MPa. [2] The composite material according to [1], wherein the aryl-containing synthetic polymer comprises polyethylene terephthalate (PET). [3] [2] The composite material according to [2], wherein the PET is contained in an amount of less than 5% of the total weight of the composite material. [4] The following features: said composite material having a density of 1.2 gr / cm 3 having a density of: - the composite material has a thermogravimetric analysis (TGA) temperature greater than 200°C; - the sample of said composite material subjected to injection molding ○ Tensile strength of at least 10 MPa, a tensile modulus of at least 1,500 MPa, A flexural modulus of at least 1,500 MPa, and a bending strength of at least 20 MPa, and -The composite material according to any one of [1] to [3], characterized by at least one of the following: -The composite material contains less than 5 mg / g of silicate. [5] 10. The composite material according to claim 1, further comprising a halogenated polymer in an amount of less than about 1% w / w of the total weight of the composite material. [6] 1.2gr / cm 3 The composite material according to any one of [1] to [5], having the following density: [7] The composite material according to any one of [1] to [6], which has a thermogravimetric analysis (TGA) temperature of more than 200°C. [8] In a sample of the composite material subjected to injection molding, the sample - Tensile strength of at least 10Mpa, - a tensile modulus of at least 1,500 MPa, a flexural modulus of at least 1,500 MPa, and The composite material according to any one of [1] to [7], having a flexural strength of at least 20 MPa. [9] The composite material according to any one of [1] to [8], which contains less than 5 mg / g of silicate.

[10] The composite material according to any one of [1] to [9], comprising micronized particles having a size distribution of d90 of 1,500 μm or less.

[11] The composite material according to any one of [1] to

[10] , comprising micronized particles having a size distribution of d90 of 900 μm or less.

[12] 1. A method for preparing a composite material, said method comprising: a. subjecting the particulate heterogeneous incorporation material to at least one extrusion process in an extruder at a temperature maintained within the range of 150°C and 200°C, thereby obtaining said composite material; The particulate foreign incorporation material is i. at least 40% w / w of non-plastic organic matter by total weight of heterogeneous waste, said non-plastic organic matter comprising at least cellulose; ii. about 5% w / w to about 60% w / w of a plastic material by total weight of the composite material, the plastic material comprising a plurality of synthetic thermoplastic polymers; iii. up to 15% w / w of inorganic material of the total weight of the composite material; The method wherein the heterogeneous incorporation material comprises an aryl-containing synthetic polymer in an amount less than 10% of the total weight of the composite material.

[13] 12. The method of claim 11, wherein the incorporation material comprises a halogenated polymer in an amount of less than about 1% w / w of the total weight of the composite material.

[14] The method according to

[12] or

[13] , wherein the aryl-containing synthetic polymer comprises PET.

[15] 14. The method of claim 13, wherein the incorporation material comprises PET in an amount less than 5% of the total weight of the composite material.

[16] The method according to any one of

[12] to

[15] , comprising subjecting the particulate heterogeneous waste to at least one separation step prior to the extrusion process, the separation step comprising removing one or both of halogenated polymers and aryl synthetic polymers from the particulate heterogeneous waste based on near-infrared (NIR) absorbance to obtain sorted heterogeneous waste.

[17] The method according to any one of

[12] to

[16] , wherein the particulate foreign material is obtained by subjecting foreign waste to two or more granulation and sieving steps.

[18] The method according to any one of

[12] to

[17] , comprising controlled slow cooling of the extrudate discharged from the extruder.

[19] The method according to any of

[12] to

[18] , wherein the composite material is subjected to at least one micronization step comprising a size reduction of the composite material.

[20]

[19] The method of

[19] , wherein the size reduction is to a size defined by a d90 of 1,500 mm or less.

[21] An article of manufacture comprising a homogeneous blend of the composite material according to any one of [1] to

[11] and at least one polyolefin.

[22] A method for producing an article of manufacture, the method comprising processing a composite material according to any one of [1] to

[11] with at least one polyolefin, the processing comprising at least one of extrusion and molding, the processing providing an intimate blend of the composite material with the at least one polyolefin. [Brief explanation of the drawings]

[0024] For a better understanding of the subject matter disclosed herein, and to illustrate how it may be carried out in practice, embodiments will now be described, by way of non-limiting example only, with reference to the accompanying drawings, in which: [Figure 1A]1A and 1B are graphs of combined thermogravimetry (TG) and differential scanning calorimetry (DSC) analyses (TG-DSC), where FIG. 1A is a DSC graph of a composite material having a particle size of approximately 1.4 mm ("Q1.4") from 0° C. to 1,500° C. at 50° increments per minute, and FIG. 1B is a DSC graph of a composite material having a particle size of approximately 0.9 mm ("Q0.9") from 0° C. to 1,500° C. at 50° increments per minute. [Figure 1B] 1A and 1B are graphs of combined thermogravimetry (TG) and differential scanning calorimetry (DSC) analyses (TG-DSC), where FIG. 1A is a DSC graph of a composite material having a particle size of approximately 1.4 mm ("Q1.4") from 0° C. to 1,500° C. at 50° increments per minute, and FIG. 1B is a DSC graph of a composite material having a particle size of approximately 0.9 mm ("Q0.9") from 0° C. to 1,500° C. at 50° increments per minute. [Figure 2] 1 is a Fourier transform infrared spectroscopy of composite materials according to the present disclosure, including a composite material having a particle size of 0.9 mm ("Q0.9") and a composite material having a particle size of 1.4 mm ("Q1.4"). DETAILED DESCRIPTION OF THE INVENTION

[0025] Producing usable composite materials from heterogeneous plastic-containing waste faces many challenges.

[0026] When different types of plastics are melted together, they tend to phase separate, like oil and water. The phase boundary causes structural weaknesses in the resulting composite material. In other words, polymer blends from recycled heterogeneous waste are only useful in limited applications. To overcome physical weaknesses, additional virgin material can be added each time heterogeneous plastic waste is recycled to help improve the integrity of the material.

[0027] It has now been discovered that certain plastics are undesirable for producing composite materials from heterogeneous plastic waste. Specifically, it is now recognized that certain synthetic plastics, such as polyvinyl chloride (PVC) and polyethylene terephthalate (PET), are considered incompatible with other plastics that are typically recycled, such as polyolefins.

[0028] In some instances, incompatibility can be defined by having a melting point above that of the recyclable polyolefin (e.g., above 200°C), and therefore may not melt sufficiently during processing of the heterogeneous waste, and therefore may behave similarly to metals and / or ceramics in composites. Without being bound by theory, plastics with melting points above the processing temperature of the heterogeneous waste appear to disrupt the homogeneity of the resulting composite, thereby structurally weakening the resulting composite. The presence of such plastics, i.e., plastics with melting points above the temperature at which the heterogeneous waste is processed, can pose challenges in forming composites for use in the recycling industry.

[0029] In some instances, incompatibility can be defined by plastics that tend to release toxic volatiles during processing of dissimilar wastes, including, for example, PVC.

[0030] Another challenge is the presence of impurities in the heterogeneous waste. The inventors of the present invention have recognized that inorganic materials, such as metals and ceramics, act as impurities because they are not miscible / soluble during the processing of the heterogeneous waste. The presence of such impurities adversely affects the homogeneity of the resulting composite material. Sometimes, these inorganic materials create "voids" in the resulting composite material, and these voids can cause structural weaknesses in the resulting composite material. Sometimes, the presence of inorganic materials also damages the equipment used to process the heterogeneous waste and produce useful, durable composite materials according to the present disclosure.

[0031] Based on the recognition that it may be advantageous to remove incompatible plastics from waste materials prior to processing, the present disclosure provides composite materials and methods for obtaining composite materials from heterogeneous waste materials (such as municipal waste) from which plastics incompatible with recyclable polyolefins have been removed (thus containing only small amounts, if any). Such processed heterogeneous waste can be considered modified heterogeneous waste. The plastics incompatible with polyolefins include at least aryl-containing synthetic polymers, such as polystyrene and PET, and optionally halogenated polymers, such as PVC. The composite materials can be molded into a variety of useful manufactured articles due to the thermoplastic behavior of the resulting composite materials. The composite materials, in turn, possess unexpectedly beneficial strength.

[0032] Thus, the present disclosure provides a composite material comprising a homogeneous blend of non-plastic organic materials, a plurality of different types of synthetic plastic materials, including a plurality of thermoplastic polymers, and inorganic materials.

[0033] In the context of the present disclosure, reference to a "homogeneous blend" should be understood to encompass a mass containing particulate material that is essentially uniformly dispersed such that any cross-section along the composite shows essentially the same appearance of the material within the continuous mass, or in other words, a mass having a substantially uniform distribution of particulate material such that any cross-section along the composite shows substantially the same appearance of membranes within the continuous mass. Furthermore, reference to a homogeneous blend should be understood to exclude composite materials that are made from or include separate layers or separate sections of different / distinguishable materials.

[0034] The composite material has defined ranges for each of these components (discussed further below), the thermoplastic polymers in the composite material contain at most 10% w / w, preferably less, of plastics that are incompatible with the polyolefin; and The polyolefin-incompatible plastic comprises at least one aryl-containing compound.

[0035] In the context of the present disclosure, as noted above, when present, the amount of aryl-containing synthetic polymer (including one or more aryl-containing synthetic polymers) is less than about 10% of the total weight of the composite material. Sometimes, the amount of aryl-containing synthetic polymer is less than about 9% w / w, sometimes less than about 8% w / w, sometimes less than about 7% w / w, sometimes less than about 6% w / w, sometimes less than about 5% w / w, sometimes less than about 4% w / w, sometimes less than about 3% w / w, sometimes less than about 2% w / w, and sometimes less than about 1% w / w.

[0036] In some examples, the polyolefin-incompatible polymer also includes one or more halogenated polymers, and in some examples, when present in the composite, the amount of halogenated polymer is less than about 1% w / w of the total weight of the composite.

[0037] In some examples, the composite materials disclosed herein have a density of 1.2 gr / cm 3 It has the following density:

[0038] In some examples, the composite materials disclosed herein have a notched Izod impact of at least 15 J / m.

[0039] In some examples, the composite material has a thermogravimetric analysis (TGA) temperature greater than 200°C.

[0040] In some examples, the composite material comprises less than 5 mg / g of silicate.

[0041] In some instances, the composite material sample subjected to injection molding may include: ○ Tensile strength of at least 8Mpa, a tensile modulus of at least 1,500 MPa, A flexural modulus of at least 1,500 MPa, a flexural strength of at least 15 MPa.

[0042] The composite materials disclosed herein may be characterized by any combination of the above features, including one, two, three, four or more of the above features, with each combination constituting a separate embodiment of the present disclosure.

[0043] In some examples, the composite material is characterized by a notched Izod of at least 15 j / m, and a tensile strength of at least 8 MPa and a flexural strength of at least 15 MPa, where the tensile strength and flexural strength are determined on an injection molded sample of the composite material.

[0044] As described above, the composite material includes a non-plastic organic material. The non-plastic organic material is present in an amount of at least about 40% w / w of the total weight of the composite material. In some examples, the non-plastic organic material is present in an amount of at least about 45%, sometimes at least about 50%, sometimes at least about 55%, sometimes at least about 60%, sometimes at least about 65%, sometimes at least about 70%, sometimes at least about 75%, sometimes at least about 80%, sometimes at least about 85%, sometimes at least about 90%, and sometimes about 95%.

[0045] In some examples, the amount of non-plastic organic material can be within any range between the above lower and upper limits, such as about 40% to 95%, e.g., about 40% to 90%, or about 50% to 85%, or about 65% to 90%, etc.

[0046] The non-plastic organic material includes at least cellulose. In some examples, the organic material may further include hemicellulose and / or lignin.

[0047] In the context of this disclosure, reference to cellulose should be understood to encompass any cellulose-containing molecule, including modified cellulose, such as paper, cardboard, vegetables, and plants, all of which are typically found in municipal waste.

[0048] The presence and amount of cellulose in the composite material can be determined using thermal analysis methods including differential scanning calorimetry (DCS, which allows for the determination of synthetic polymer content) and thermogravimetric analysis (TGA, which allows for the determination of lignocellulose content and inorganic content).

[0049] As mentioned above, the composite material comprises a plastic material, which comprises a plurality of synthetic thermoplastic polymers and optionally thermosetting polymers.

[0050] The plastic material is present in an amount of at least about 5% w / w of the total weight of the composite, sometimes at least about 6%, sometimes at least about 7%, sometimes at least about 8%, sometimes at least about 9%, sometimes at least about 10%, sometimes at least about 11%, sometimes at least about 15%, sometimes at least about 20%, sometimes at least about 25%, sometimes at least about 30%, and sometimes at least about 35%.

[0051] The plastic material is present in an amount of up to about 60% w / w of the total weight of the composite, sometimes up to about 55%, sometimes up to about 40%, sometimes up to about 35%, sometimes up to about 30%, sometimes up to about 25%, sometimes up to about 20%, sometimes up to about 15%, and sometimes up to about 12%.

[0052] In some examples, the amount of plastic material can be within any range between the above lower and upper limits, such as about 5% to 60%, e.g., about 8% to 50%, about 5% to 30%, about 8% to 30%, or about 10% to 40%, or about 10% to 30%, or about 5% to 15%, etc.

[0053] The plastic materials in the composite material are heterogeneous. In this regard, it should be understood that the plastic material may not consist solely of virgin plastic or plastics of similar properties, such as one or more polyolefins. Thus, in the context of the present disclosure, the plastic material should be understood to include one or more polyolefins and at least one other non-olefin polymer.

[0054] In some examples, the non-olefin polymer contains no, less than 10%, or even less than 5% aryl-containing compounds (ie, aryl-containing synthetic polymers).

[0055] In some examples, the non-olefin polymer contains no or less than 1% halogenated polymer, specifically no or less than 1% PVC.

[0056] In some examples, the composite material has less than 10% w / w of polymer with a melting point range of at least 200° C. Sometimes the composite material contains less than 9% w / w, or less than 8% w / w, or less than 7% w / w, or less than 6% w / w, or less than 5% w / w, or less than 4% w / w, or less than 3% w / w, or even less than 2% w / w of polymer with a melting point range of at least 200° C. or greater.

[0057] In some examples, the plastic material in the composite other than polyolefin (ie, the non-polyolefin polymer) comprises polyacrylonitrile.

[0058] In some examples, the plastic material in the composite other than polyolefin (ie, the non-polyolefin polymer) comprises polybutadiene.

[0059] In some examples, the plastic material in the composite other than polyolefin (ie, the non-polyolefin polymer) comprises polycarbonate.

[0060] In some examples, the plastic material in the composite other than polyolefin (ie, the non-polyolefin polymer) comprises polyamide (PA).

[0061] In some examples, the plastic material in the composite other than polyolefin (ie, the non-polyolefin polymer) comprises ethylene vinyl alcohol copolymer (EVOH).

[0062] In some examples, the plastic material in the composite other than polyolefin (ie, the non-polyolefin polymer) comprises polyurethane (PU).

[0063] In some examples, the plastic material in the composite other than polyolefin (i.e., the non-polyolefin polymer) includes polyethylene terephthalate (PET), but as noted above, PET is present in an amount less than 10% w / w, or less than 9% w / w, or less than 8% w / w, or less than 7% w / w, or less than 6% w / w, or less than 5% w / w, or less than 4% w / w, or less than 3% w / w, or even less than 2% w / w.

[0064] In some instances, the plastic material includes at least two types of polyolefin, such as high density polyethylene (HDPE), low density polyethylene (LDPE), and polypropylene (PP).

[0065] A composite material comprises a heterogeneous blend of plastics, and therefore comprises at least one polyolefin and at least one non-olefin compound. Preferably, the composite material comprises multiple (more than two) polyolefin plastics and multiple (more than two) non-polyolefins.

[0066] In some instances, the plastic material comprises a thermoset resin, although it constitutes only a small portion of the composite. In some instances, the plastic material comprises up to 1% thermoset resin. Some non-limiting examples of thermoset resins that may be present in the composite include vulcanized rubber, vulcanized thermoplastic polymers (TPV), and / or polyurethane (PU).

[0067] As noted above, the composite material can include inorganic material, which is present in an amount of up to about 15% w / w, sometimes up to about 10%, sometimes up to 9%, sometimes up to 8%, sometimes up to 7%, sometimes up to 6%, sometimes up to 5%, and sometimes up to about 4%, 3%, 2%, or even 1%.

[0068] In some examples, the amount of inorganic material can be within any range between the above lower and upper limits, such as about 1% to 15%, for example, about 5% to 10%, or about 1% to 10%, or about 3% to 8%, etc.

[0069] In some examples, inorganic materials in composite materials refer to materials typically found in municipal, domestic, and / or industrial waste streams, including, but not limited to, sand, stone, glass, ceramics, and other minerals, as well as metals, including, for example, aluminum, iron, and copper.

[0070] In some examples, the inorganic material includes silicate in amounts discussed further below.

[0071] In the context of this disclosure, reference to composite materials lacking detectable amounts of certain synthetic plastics or having amounts below a specified range should be understood as a determination made using conventional analytical techniques.

[0072] In one example, the composite material can be characterized as having no or only a negligible amount of halogenated polymer that can be detected.

[0073] In some examples, the composite material can be characterized as having no detectable amount or a trace amount (less than about 10% w / w, or less than 9% w / w, or less than 8% w / w, or less than 7% w / w, or less than 6% w / w, or less than 5% w / w, or less than 4% w / w, or less than 3% w / w, or less than 2% w / w) of the aryl-containing synthetic polymer. The presence (trace amount) or absence of a detectable amount of the aryl-containing synthetic polymer in the composite material can be determined using NIR techniques, such as the systems disclosed herein.

[0074] In the context of the present disclosure, reference to an "aryl-containing synthetic polymer" or "aryl-containing compound" should be understood to refer to a high molecular weight compound, preferably comprising a polymer that contains an aryl-containing organic moiety as a monomer unit of the polymer.

[0075] In some examples, the aryl group of the aryl-containing organic compound comprises a phenyl group.

[0076] In some other examples, the aryl group of the aryl-containing organic compound comprises a styrene group.

[0077] In preferred examples, the aryl-containing organic compound includes polymers such as, but not limited to, polystyrene, high impact polystyrene (HIPS), acrylonitrile butadiene styrene (ABS), polyethylene terephthalate (PET), and the like, each example being considered an independent aspect of this disclosure.

[0078] In some examples, the aryl-containing synthetic polymer includes or is polystyrene.

[0079] In some examples, the aryl-containing synthetic polymer includes at least PET.

[0080] As shown in the non-limiting examples, after NIR treatment the waste contains less than twice the amount of PET than without NIR treatment.

[0081] In some instances, NIR treatment is also used to remove halogenated polymers. In the context of the present invention, the term "halogenated polymer" encompasses any synthetic plastic polymer, such as PVC and fluorinated ethylene propylene (FEP), derived from fluorine. Specifically, composite materials can be characterized as having no detectable amount of PVC or only a small amount of PVC. The presence or absence of halogenated polymers, particularly PVC, in composite materials can be detected using near-infrared (NIR) techniques. In some instances, halogenated polymers, particularly PVC, are detected using an NIR system such as a SESOTEC MN 1024, which is further discussed below in the Examples section, which forms an integral part of this disclosure.

[0082] In some examples, the composite materials disclosed herein have been shown to have one or any combination of beneficial physical characteristics, including density, notched Izod impact, characteristic thermogravimetric analysis profile (TGA), tensile strength, tensile modulus, flexural modulus, and flexural strength, among others.

[0083] In some instances, composite materials are defined by having a particular density level. In the context of this disclosure, when referring to density, it is understood that a composite material may have a density of 1.2 gr / cm 2 It should be understood that: Without being bound by theory, this density may result from limiting and / or eliminating the amount of inorganic materials (metal, glass, silica, etc.). As shown in the non-limiting examples, the disclosed technology provides lighter weight composite materials compared to those of WO 2010 / 082202, which is believed to be a commercial benefit (e.g., in terms of cost per volume).

[0084] The density can be determined using density ISO 1183-1 (ASTM D792 procedure), as further described below in connection with the Examples which form an integral part of this disclosure.

[0085] In some other instances, the composite material is defined by its notched Izod impact. In the context of this disclosure, when referring to the notched Izod impact of the composite materials disclosed herein, it should be understood to be at least 15 J / m.

[0086] Without limitation, notched Izod impact, which is a measure of a composite material's resistance to impact from a pendulum, can be determined using ASTM D256 (ISO 180), as further described below in connection with the Examples that form an integral part of this disclosure.

[0087] In some examples, the notched Izod impact of the composite is at least 16 J / m, sometimes at least 17 J / m, sometimes at least 18 J / m, sometimes at least 19 J / m, sometimes at least 20 J / m, sometimes at least 21 J / m, sometimes at least 22 J / m, sometimes at least 23 J / m, sometimes at least 24 J / m, sometimes at least 25 J / m, and sometimes at least 26 J / m.

[0088] In some instances, the notched Izod impact is within the range of 15 J / m and 50 J / m, sometimes within the range of 20 J / m and 40 J / m, sometimes within the range of 20 J / m and 35 J / m, sometimes within the range of 18 J / m and 40 J / m, and sometimes within the range of 15 J / m and 35 J / m.

[0089] In some examples, the composite material is characterized by a specific thermogravimetric analysis (TGA) with a weight loss of greater than 5% at temperatures above 200°C, sometimes above 210°C, and sometimes above 215°C. As will be appreciated, TGA measures weight loss as a function of temperature. A 5% loss indicates the onset of decomposition. The composite material disclosed herein has been found to be more stable than waste-derived composite materials such as those described in WO 2010 / 082202 (the "reference composite material"), which had an upper temperature limit of <200°C. As will be appreciated, the higher the temperature at which there is a weight loss of greater than 5%, the more stable the material (which means a wider processing temperature window is achieved). For example, in the non-limiting examples provided herein, two samples of the composite material disclosed herein (Q0.9 and Q1.4) have TGA temperatures above 210°C (218°C and 224°C, respectively), which is higher than that of the reference composite material, which is 170°C.

[0090] TGA can be provided using thermogravimetry-differential scanning calorimetry as described below in the Examples section which forms an integral part of this disclosure.

[0091] Generally, as understood by those skilled in the art, TGA uses heat to force reactions and physical changes in materials. It provides quantitative measurements of the mass change of a material associated with transformations and thermal decomposition. TGA records the change in mass from the dehydration, decomposition, and oxidation of a sample over time and temperature. Characteristic thermogravimetric curves are generated for specific materials and chemical compounds due to the unique sequence of physicochemical reactions that occur over a specific temperature range and heating rate. These unique characteristics are related to the molecular structure of the sample. DSC is a thermal analysis technique that measures the heat flow to or from a sample as a function of temperature or time while the sample is exposed to a controlled temperature program. It allows for the evaluation of material properties such as glass transition temperature, melting, crystallization, specific heat capacity, curing process, purity, oxidation behavior, and thermal stability.

[0092] Composite materials can also be characterized by their tensile properties, which are determined from injection-molded specimens prepared from the composite material. For example, specimens for determining the physical properties of the composite material can be prepared by subjecting a quantity of the composite material to the following injection molding conditions: Preparation of test specimens for injection molding can include melting the extrudate at 170-180°C and 350 rpm in an extruder, granulating the extrudate into essentially uniformly sized granules, and injection molding the granules in an injection molder at 170-180°C to obtain the test specimens. Test specimens were conditioned at 23±2°C for at least 48 hours.

[0093] Measurement of tensile properties of injection-molded samples can be provided using ISO 521-2:1996. According to ISO 521-2, specimen type 1A can be used at a test speed of 50 mm / min, with the following dimensions: total length ≥ 150-200 mm, narrow parallel-sided length = 80 ± 2 mm, radius 20-25 mm, distance between wide parallel-sided portions 104-113 mm, width at the ends = 20 ± 0.2 mm, width at narrow portion 10 ± 0.2 mm, preferred thickness 4 ± 0.2 mm, gauge length 50 ± 0.5 mm, and initial distance between grips = 115 ± 1 mm.

[0094] According to some examples, the composite material can be characterized by a tensile strength of at least 8 MPa.

[0095] In some further examples, injection molded samples of the composite material have a tensile strength of at least 9 MPa, sometimes at least 10 MPa, sometimes at least 11 MPa, sometimes at least 12 MPa, and sometimes at least about 13 MPa.

[0096] In some further examples, the tensile strength of an injection molded sample of the composite is at most 25 MPa, at most 22 MPa, or at most 20 MPa.

[0097] In some examples, the tensile modulus of an injection molded sample of the composite is at least 1,500 MPa, sometimes at least 1,600 MPa, sometimes at least 1,700 MPa, sometimes at least 1,800 MPa, sometimes at least 1,900 MPa, sometimes at least 2,000 MPa, and sometimes at least 2,100 MPa.

[0098] In some instances, the tensile modulus of an injection molded sample of the composite is at most 3,000 MPa.

[0099] The composite material may also be characterized by its flexural properties, which may be measured in accordance with ISO 178. In accordance with ISO 178, the specimen dimensions were length = 80 ± 2 mm, width = 10 ± 0.2 mm, and thickness = 4 ± 0.2 mm. Also in accordance with ISO 178, the test speed was 5 mm / min. Typically, the test results were the average of measurements on at least five specimens, as discussed further below.

[0100] In some examples, an injection molded sample of the composite has a flexural modulus of at least 1,500 MPa, sometimes at least 1,600 MPa, sometimes at least 1,700 MPa, sometimes at least 1,800 MPa, sometimes at least 1,900 MPa, sometimes at least 2,000 MPa, sometimes at least 2,100 MPa, sometimes at least 2,200 MPa, sometimes at least 2,300 MPa, sometimes at least 2,400 MPa, sometimes at least 2,500 MPa, sometimes at least 2,600 MPa, and sometimes at least 2,700 MPa.

[0101] In some instances, the flexural modulus of an injection molded sample of the composite material is at most 7,000 MPa, sometimes at most 6,000 MPa, sometimes at most 5,000 MPa, sometimes at most 4,000 MPa, and sometimes at most 3,000 MPa.

[0102] In some instances, the flexural strength of an injection molded specimen of the composite is at least 15 MPa, sometimes at least 16 MPa, sometimes at least 17 MPa, sometimes at least 18 MPa, sometimes at least 19 MPa, sometimes at least 20 MPa, sometimes at least 21 MPa, sometimes at least 22 MPa, sometimes at least 23 MPa, and sometimes at least 24 MPa.

[0103] In some instances, injection molded samples of the composite have a flexural strength of at most 50 MPa, sometimes at most 40 MPa, and sometimes at most 30 MPa.

[0104] Without limitation, flexural strength was determined in accordance with ISO 178. According to ISO 178, test specimens with the following dimensions are prepared: length = 80 ± 2 mm, width = 10 ± 0.2, thickness = 4 ± 0.2 mm. Test conditions include a test speed of 5 mm / min. In the following examples, at least five test specimens were tested using a Tinius Olsen H10KT instrument. The test results were the average of these measurements.

[0105] The composite materials disclosed herein can also be characterized by the amount of silicate. According to some examples, the amount of silicate is less than 10 mg / g. The amount of silicate and other inorganic elements can be determined using an argon plasma in the technique of inductively coupled plasma atomic emission spectroscopy (ICP-AES), details of which are provided in the following examples, which form an integral part of this disclosure.

[0106] In some examples, the amount of silica in the composite is at most 7 mg / g, sometimes at most 6 mg / g, sometimes at most 5 mg / g, sometimes at most 4 mg / g, sometimes at most 3 mg / g, sometimes at most 2 mg / g, and sometimes at most 1 mg / g.

[0107] In some instances, the composite material does not contain detectable amounts of silica. Sometimes the composite material contains 0.1-5 mg / g silica, sometimes 1 mg / g-10 mg / g silica, sometimes 5 mg / g-10 mg / g silica, sometimes 0.5 mg / g-2 mg / g, sometimes any range between 1 mg / g-10 mg / g.

[0108] In some instances, the composite material can be characterized by its surface energy, which is determined according to ASTM D2578-84 using a commonly known, commercially available Dyne Test Pen. In some instances, the surface energy is greater than 35 dynes / cm, sometimes greater than about 36 dynes / cm. Sometimes, the surface energy is between 35 and 40 dynes / cm.

[0109] A composite material can also be characterized by its flame retardancy or flammability as defined by its Limited Oxygen Index (LOI) ISO 4589-2:2017. In some instances, a composite material is defined by an LOI of up to 21.5%. For comparison, the LOI of PE or PP is equal to 17, meaning these polymers are more flammable.

[0110] The composite materials of the present disclosure can also be characterized for the presence of DNA material as detected using a chloroform:isoamyl alcohol (24:1) (CTAB) solution in a conventional DNA extraction protocol, as described, for example, by Yi, S., Jin, W., Yuan, Y. and Fang, Y. (2018). An Optimized CTAB Method for Genomic DNA Extraction from Freshly-picked Pinnae of Fern, Adiantum capillus-veneris L. Bio-protocol 8(13):e2906. DOI: 10.21769 / BioProtoc.2906 (see also the Examples, which form an integral part of this disclosure).

[0111] The composite materials of the present disclosure can also be characterized by the presence of chlorophyll, as detected using conventional protocols, as described, for example, by Yi, S., Jin, W., Yuan, Y. and Fang, Y. (2018). An Optimized CTAB Method for Genomic DNA Extraction from Freshly-picked Pinnae of Fern, Adiantum capillus-veneris L. Bio-protocol 8(13):e2906. DOI: 10.21769 / BioProtoc.2906 (see also the Examples, which form an integral part of this disclosure).

[0112] The composite materials of the present disclosure may also be characterized by the presence of 1.5 mg / g or less of ferrous (Fe) material as determined using ICP-AES, as described herein.

[0113] The composite materials of the present disclosure may also be characterized by the presence of sodium (Na) of 5 mg / g or less, sometimes even 4 mg / g or less, or even 3 mg / g or less, or even 2 mg / g or less, as determined using ICP-AES, as described herein.

[0114] The composite materials of the present disclosure may also be characterized by the presence of less than or equal to 5 mg / g Al, and sometimes even less than or equal to 4 mg / g Al, as determined using ICP-AES as described herein.

[0115] The composite materials of the present disclosure may also be characterized by the presence of potassium of 5 mg / g or less, sometimes 4 mg / g or less, sometimes even 3 mg / g or less, or even 2.5 mg / g or less, as determined using ICP-AES, as described herein.

[0116] The composite materials of the present disclosure may also be characterized by the presence of magnesium (Mg) of 5 mg / g or less, sometimes 4 mg / g or less, sometimes even 3 mg / g or less, or even 2.5 mg / g or less, as determined using ICP-AES, as described herein.

[0117] Composite materials can be prepared from heterogeneous waste materials. In the context of this disclosure, when referring to "heterogeneous waste materials," it should be understood as materials that include a heterogeneous blend combination of synthetic plastic materials, non-plastic organic materials including at least cellulose, and inorganic materials.

[0118] For purposes of producing the composite materials disclosed herein, the blend of synthetic plastic materials comprises a plurality of polymers, the plurality of polymers containing less than 10% w / w of an aryl-containing synthetic polymer.

[0119] In some examples, the synthetic polymer blend (1) lacks detectable amounts of plastics that are incompatible with polyolefins or contains insignificant amounts (i.e., less than 10% w / w) of plastics that are incompatible with polyolefins, and / or (2) lacks detectable amounts of halogenated polymers such as polyvinyl chloride (PVC) or contains insignificant amounts of halogenated polymers such as PVC, where insignificant amounts are less than about 1% w / w of the total weight of the composite material, and / or (3) lacks detectable amounts of aryl-containing synthetic polymers or contains insignificant amounts of aryl-containing synthetic polymers, where insignificant amounts are less than about 10%, preferably less than 5% w / w, or more preferably less than 4% w / w, as defined above. Heterogeneous waste materials containing blends of synthetic plastic materials that contain insignificant amounts of incompatible plastics as defined above or that further lack detectable amounts of incompatible plastics are referred to herein as heterogeneous incorporation materials.

[0120] The heterogeneous waste, prior to removal of polyolefin-incompatible plastics (preferably PET), can be obtained from municipal, industrial, and / or domestic waste. This heterogeneous waste is then subjected to a sorting process to provide a heterogeneous incorporation material containing a plurality of heterogeneous plastic materials, non-plastic organic materials, and inorganic materials, but, as described above, containing less than 10% aryl-containing synthetic polymers (e.g., PET).

[0121] The heterogeneous incorporation material is particulate to form a particulate heterogeneous incorporation material, which is then processed into a product. The product can constitute an ingredient for the production of an article of manufacture, or the product is a final product, i.e., a useful article of manufacture.

[0122] Thus, the present disclosure provides a method of producing a composite material from heterogeneous incorporation materials according to the present disclosure that can produce a useful article of manufacture, the incorporation materials comprising: i. at least 40% w / w of a non-plastic organic material of the total weight of the heterogeneous incorporation material, the non-plastic organic material comprising at least cellulose; ii. about 5% w / w to about 60% w / w of a plastic material of the total weight of the heterogeneous incorporation material, the plastic material comprising a plurality of thermoplastic polymers; iii) up to 15% inorganic material by weight of the total heterogeneous incorporation material.

[0123] In one example, the method disclosed herein comprises subjecting a heterogeneous incorporation material as defined above to at least one extrusion process under conditions comprising an internal (operating) temperature of about 150°C to about 200°C, thereby obtaining said composite material; The plurality of thermoplastic polymers comprises an aryl-containing synthetic polymer in an amount less than 10% w / w of the total weight of the composite, sometimes even less than 9% w / w, sometimes even less than 8% w / w, sometimes even less than 7% w / w, sometimes even less than 6% w / w, and sometimes even less than 5% w / w of the total weight of the composite.

[0124] In some examples, the composite material includes less than 10% w / w of a plastic that is incompatible with the polyolefin, with a maximum amount of 10% w / w including at least PET.

[0125] The foreign incorporation material is either granulated prior to extrusion or fed to the extruder in granular form.

[0126] In some examples, at least one extrusion process also includes a residence time in the extruder of at least 4 minutes, sometimes at least 5 minutes, and preferably at least 5.5 minutes. This residence time is particularly relevant when the extruder is a single-screw extruder. In this regard, it should be noted that when using a twin-screw extruder, shorter residence times can be applied. However, a single-screw extruder and a long residence time (greater than 4 minutes) are preferred.

[0127] In yet some other examples, the particulate heterogeneous incorporation material subjected to at least one extrusion process comprises a plurality of thermoplastic polymers including a minor amount of an aryl-containing synthetic polymer, such as polystyrene, the minor amount being less than about 10%, sometimes less than about 9%, sometimes less than about 8%, sometimes less than about 7%, sometimes less than about 6%, sometimes less than about 5%, sometimes less than about 4%, and sometimes less than about 3%.

[0128] In some examples, the particulate heterogeneous incorporation material subjected to at least one extrusion process comprises multiple thermoplastic polymers including a minor amount of a halogenated polymer, such as polyvinyl chloride (PVC), the minor amount being less than about 1% w / w of the total weight of the composite material.

[0129] In yet another example, the method of the present disclosure includes subjecting the particulate foreign incorporation material to a separation step that includes removing polymers having a melting point above 200°C.

[0130] In some further examples, the methods of the present disclosure include subjecting the particulate foreign incorporation material to a separation step that includes removal of polyvinyl chloride.

[0131] In some further examples, the methods of the present disclosure include subjecting the particulate heterogeneous incorporation material to a separation step that includes removing one or more aryl-containing synthetic polymers from the particulate heterogeneous incorporation material based on near-infrared (NIR) absorbance to obtain sorted heterogeneous waste.

[0132] The heterologous incorporation material is provided in particulate form.

[0133] According to some examples, the heterogeneous incorporation material is obtained from heterogeneous unsorted waste that is a priori subjected to one or more pre-treatment steps of the raw heterogeneous unsorted waste that ultimately results in a particulate incorporation material suitable for the methods disclosed herein.

[0134] In the context of the present disclosure, the term "raw heterogeneous waste" or "raw waste" for short refers to heterogeneous waste material that has not been sorted, i.e., has not been subjected to any industrial sorting process.

[0135] In some examples, the raw heterogeneous waste material undergoes a pre-sorting process in which large, undesirable waste items are removed. For example, the raw waste can be pre-sorted to remove any one of metals, glass, and large minerals. Pre-sorting can be performed manually, for example, by transporting the raw waste on a conveyor belt and identifying large, undesirable waste items.

[0136] Additionally or alternatively, pre-sorting typically involves separation using magnetic forces (magnet-based separation) for the separation and removal of ferrous metals.

[0137] Additionally or alternatively, pre-sorting typically involves separation using an eddy current separator for removal of non-ferrous metals.

[0138] The waste material can also be subjected to a drying process. In the context of this disclosure, reference to drying should be understood as removing a portion of the water from the waste material. Drying should not be interpreted as removing all of the water from the waste. In some instances, raw waste contains about 30%-40% w / w water, and drying involves removing at least 50% of the water content, sometimes at least 60% of the water content, sometimes at least 70% of the water content, sometimes at least 80% of the water content, sometimes at least 90% of the water content, and sometimes at least 95% of the water content. The resulting waste material can then be considered dry waste material.

[0139] In some instances, the dry waste material contains at most 11% w / w water, at most 10% w / w water, sometimes at most 9% water, sometimes at most 8% water, sometimes at most 7% water content, and sometimes at most 6% water content.

[0140] Drying can be accomplished by any means known in the art.

[0141] In some instances, drying is achieved by placing the waste outside and letting it dry, while in some other instances, drying is achieved by placing the waste under a dry air stream and / or in an oven chamber and / or by squeezing out the liquid.

[0142] The drying process removes water and sometimes some volatile liquids, which may include liquids with a vapor pressure of at least 15 mmHg at 20°C, such as ethanol.

[0143] In some instances, drying is accomplished by a biodrying process that utilizes bacteria naturally present in the waste. To this end, the waste material is typically placed in a temperature-controlled environment. In some instances, biodrying is carried out at a temperature maintained at about 70°C.

[0144] In some instances, bacteria are added to waste materials (eg, pre-sorted waste materials) to induce or enhance the biodrying process.

[0145] Without wishing to be bound by theory, it is presently believed that any remaining residual moisture content plays a role in the chemical processes that result in the conversion of the dry waste material into the composite materials of the present disclosure.

[0146] The waste material, preferably dry waste material, is then subjected to a particulate step to obtain the particulate waste material utilized in the methods disclosed herein.

[0147] In the context of this disclosure, the term "particulation" should be understood to encompass any process involving size reduction of waste material. Particulation can occur by any one or combination of granulation, shredding, chopping, dicing, cutting, crushing, disintegration, grinding, etc.

[0148] In some instances, granulating involves shredding the waste (dry or non-dry, more preferably dry) into particles having an average size of less than 40 mm, sometimes less than 30 mm, and sometimes less than 20 mm.

[0149] Notably, due to friction within the shredder, granulation can result in further moisture loss (e.g., an additional 2% to 3%).

[0150] In some preferred examples, the particulate waste is then subjected to a selective separation process (also called a washing process) in which residual metal and / or mineral particles ("impurities") are removed.

[0151] In some examples, remaining impurities are removed by subjecting the particulate matter to an air separation system where heavier particles (e.g., metal particles and / or minerals) are removed by gravity while lighter waste fractions are collected and / or conveyed to the next process step.

[0152] The resulting light fraction will contain small amounts of metals and minerals. Without being bound thereto, it is believed that the fraction contains at most 1% w / w metals (ferrous and non-ferrous) and at most 5% minerals.

[0153] One feature of the disclosed method involves processing waste materials for selective separation using near-infrared (NIR). NIR-based separation allows for the optical separation of undesired plastic materials from other plastic waste based on polymer type (based on the wavelength signature of the resin). As will be understood by those skilled in NIR technology, NIR-based separation systems are programmed to identify many polymers and other compounds. The system operator defines which compounds are retained and which are sorted. More specifically, the NIR separation step utilizes a system equipped with an algorithm for each substance to be removed, including polymers incompatible with polyolefins, e.g., polymers with melting points above 200°C or even above 210°C, and / or halogenated and / or aryl-containing synthetic polymers, and optionally other polymers, as desired. This algorithm allows for the identification and separation of each compound accordingly. In this regard, those skilled in the art will understand that each chemical has a complex IR spectrum, which is the chemical's "fingerprint" identity. This fingerprint can be found in any publicly available "Chemical Atlas" and recognized by computer programs.

[0154] In some instances, as already mentioned above, the NIR-based separation operates in a manner that allows for the separation of at least polymers that are recognized in the art as being incompatible with polyolefins.

[0155] In some instances, as already mentioned above, the NIR-based separation is operated in a manner that allows for the separation of at least halogenated polymer resins, such as polyvinyl chloride (PVC or vinyl) resins.

[0156] In some additional or alternative examples, as already mentioned above, the NIR-based separation is operated in a manner that allows for the separation of aryl-containing synthetic polymers, preferably styrene or polystyrene organic polymers.

[0157] In some further examples, the heterogeneous incorporation material is characterized by its ash level, hi some examples, the ash content in the heterogeneous incorporation material is less than 10% w / w, sometimes less than 8% w / w, sometimes less than 6% w / w, or even less than 5% w / w.

[0158] Ash levels in the entrapped material (and final composite) can be determined according to ISO 3451 Method A using two test portions of 5 gr each, burned at 950±500°C for 30 minutes.

[0159] The resulting particulate and sorted waste material is referred to herein by the term "heterogeneous loaded material" or sometimes by the term "sorted heterogeneous loaded material."

[0160] The heterogeneous incorporation material is then subjected to at least one extrusion process. The extrusion conditions include at least: Internal (operating) temperatures below -200°C, sometimes about 150°C to about 200°C, sometimes about 120°C to about 180°C, sometimes 160°C to 200°C, sometimes 150°C to 180°C, A minimum residence time in the extruder of at least 2.0 minutes, sometimes at least 2.5 minutes, sometimes at least 3 minutes, sometimes at least 3.5 minutes, sometimes at least 4 minutes, sometimes at least 4.5 minutes, sometimes at least 5 minutes, sometimes at least 5.5 minutes, sometimes at least 6 minutes, and sometimes at least 7 minutes. However, there is a limit to the residence time that does not cause decomposition or combustion of the materials within the extruder. Thus, in some cases, the residence time is defined to be within the range of about 2 to about 10 minutes, sometimes about 3 to 7 minutes, sometimes between about 2.5 and 10 minutes, sometimes about 3.5 to 8 minutes, sometimes about 4.5 to 8 minutes, sometimes about 5.5 to 7 minutes, and sometimes about 5.5 to 6.5 minutes.

[0161] An extruder typically comprises a heated barrel containing a rotating single or multiple screws therein. There are various types of extrusion that can be used in the context of the present disclosure.

[0162] Without being bound by theory, it is believed that the application of shear forces to sorted heterogeneous waste materials at material temperatures below 200°C converts the organic fibrous materials (lignin, cellulose, hemicellulose, and other carbohydrates) into partially carbonized lignocellulosic fibers that act as a natural "molecular stitch" unifying (binding) plastic, particularly polyolefins with different polarities that would otherwise phase separate, creating an organic-thermoplastic composite.

[0163] In some preferred examples, extrusion is carried out in a single screw extruder. When using a single screw extruder, it has been found that the minimum residence time should be at least 3 minutes, or at least 4 minutes, preferably at least 5 minutes or 5.5 minutes.

[0164] In some instances, the single screw extruder has dimensions designed to allow for residence times in the ranges defined above. Those skilled in the art will know how to design the extruder diameter, length, die opening, etc. to achieve the desired residence time.

[0165] In some instances, extruders are designed to operate at 30-10 rpm, sometimes 40-90 rpm.

[0166] The operating temperature within the extrusion (ie the internal temperature, in other words the temperature of the material being extruded) can be controlled by a thermocouple, such as a type J thermocouple.

[0167] In some examples, the extruder is equipped with at least two or more ventilation zones. The presence of two separate ventilation zones along the extruder reduces the amount of volatile organic compounds in the extruded material and prevents the entrapment of volatile compounds. The presence of at least two ventilation zones has been found to be important for avoiding bubbles in manufactured articles (molded or extruded) made from the disclosed composite materials.

[0168] Various additives can be added to the heterogeneous incorporation material prior to extrusion, including, but not limited to, any one or combination of zinc stearate, calcium stearate, antioxidants, UV stabilizers, blowing agents, plasticizers, elastomers, fillers such as talc and calcium carbonate, flame retardants and pigments such as carbon black, titanium dioxide and other pigments used in the plastics industry.

[0169] The composite material exiting the extruder can then be subjected to further processing.

[0170] In some instances, the extrudate is subjected to controlled cooling.

[0171] In some instances, cooling is by subjecting the extrudate to a stream of cooling air. In some further instances, controlled cooling is by passing the extrudate on a conveyor and subjecting it to a stream of cooling air as it is conveyed. Because the cooling is gradual, it allows for further elimination of odors and VOCs.

[0172] In some instances, the composite material exiting the extruder is subjected to at least one micronization step involving size reduction of the composite material, typically after the exiting composite material has cooled.

[0173] In some instances, micronization involves milling the composite material using any conventional milling system.

[0174] In some instances, milling involves passing the composite material through a continuous milling process, such as a hammer mill (e.g., Type 40 / 32 HA).

[0175] In some other instances, the extrudate is subjected to an impact milling process in which high speed rotating blades (beater plates) pulverize the composite material against the enclosure and against itself, with friction causing a reduction in size.

[0176] In some instances, reduction can be achieved by subjecting the composite material to a "knife mill," such as that achieved by using a ROTOPLEX 50 / 100. This technology is designed to obtain high cutting forces at high throughput. Using the "scissors" principle, a drum with knives moves at high speed in front of a counter knife in a cooled environment.

[0177] In some instances, the reduction is achieved by a combination of two or more reduction techniques, for example, one utilizing a hammer mill technique and a second utilizing an impact milling technique. The combination of techniques allows for the reduction of powder cider to less than 1.5 mm.

[0178] In some instances, the extrudate was subjected to size reduction using a combination of milling equipment configured to grind the extrudate into powder (micronized composite material) and sieving through a 900 μm (0.9 mm) or 1400 μm (1.4 mm) sieve to obtain two populations of powder, one having a particle size of less than 0.9 mm (referred to herein as the abbreviation "Q0.9") and the other having a particle size of less than 1.4 mm (referred to herein as the abbreviation "Q1.4").

[0179] In some instances, the resulting powder is sieved using, for example, a vibrating sieving system that sieves particle size by using different sized holes of different diameters.

[0180] In some instances, the size reduction is to a particle size defined by a d90 of 1.4 mm or less. Sometimes the size reduction is to a particle size of 1.3 mm or less, sometimes 1.2 mm or less, sometimes 1.1 mm or less, sometimes 1.0 mm or less, sometimes 0.9 mm or less, sometimes 0.8 mm or less, and sometimes 0.7 mm or less.

[0181] In the following non-limiting examples, a refined composite material having a size of d90≦1.4 μm is referred to as the abbreviated Q1.4, and a refined composite material having a size of d90≦0.9 mm is referred to as the abbreviated Q0.9.

[0182] The resulting composite material, and preferably the refined composite material, can be reheated to a thermoplastic melt by heating to a temperature above 100° C. In some instances, the composite material will convert to a flowable melt when heated to any temperature above 120° C., sometimes above 130° C., sometimes above 140° C., sometimes above 150° C., sometimes above 160° C., sometimes above 170° C., even above 180° C., and sometimes below 200° C., provided the composite material does not undergo any decomposition or combustion as a result of the heating.

[0183] The melt can then be molded into the desired article of manufacture using any known molding technique, including extrusion injection, blow molding, and rotational molding, among others. In this manner, articles of defined configuration can be produced. For example, the composite material can be used to produce a variety of articles of manufacture, typically prepared from virgin or recycled plastics. These include, for example, flower pots, house siding, decking, flooring, furniture, laminates, pallets, septic tanks, and the like.

[0184] Various additives, fillers, etc., can be added to the composite material during reheating / reprocessing into a useful article of manufacture to impart specific desired properties to the final article after cooling. Examples of fillers include, but are not limited to, sand, minerals, recycled tire material, concrete, glass, wood chips, thermoset materials, other thermoplastic polymers, gravel, metal, glass fiber, and particles. These fillers may be derived from recycled products, but virgin materials such as virgin plastics (e.g., polypropylene and / or polyethylene) may also be used. Other additives, such as colorants, odor masking agents (e.g., activated carbon), oxidizing agents (e.g., potassium permanganate), or antioxidants, may be added to improve the appearance, texture, or scent of the composite material. Nevertheless, it should be noted that the properties of the composite material of the present disclosure and its potential applications are achieved without the need for binders or plasticizers, although these may be added under some embodiments.

[0185] Composite materials can be combined with amounts of plastic, including recycled and virgin plastic, to create an article of manufacture.

[0186] In some instances, the composite material is reheated with a polyolefin. In some instances, the composite material is reheated with one of polyethylene and polypropylene. The reheated mixture can be extruded into mixed pellets that are then used as an incorporation material in the plastics industry.

[0187] Thus, the composite materials of the present disclosure, and materials obtained by mixing the composite materials with plastics, can be processed by various industrial processes known per se to form various semi-finished or finished products.

[0188] As used herein, the forms "a," "an," and "the" include the singular and the plural unless the context clearly dictates otherwise. For example, the term "particulate material" includes one or more types of particulate material having the recited characteristics.

[0189] Furthermore, as used herein, the term "comprising" is intended to mean that the composite material includes the recited components, i.e., non-plastic organics, plastics, and inorganics, but does not exclude other elements. The term "consisting essentially of" is used, for example, to define a composite material that includes the recited elements, but excludes other elements that may have essential significance to the properties of the composite material. Thus, "consisting of" is intended to mean excluding more than trace amounts of other elements. Embodiments defined by each of these transition terms are within the scope of the present invention.

[0190] Furthermore, all numerical values, e.g., amounts or ranges of components making up the composite or heterogeneous incorporation materials disclosed herein, are approximations that may vary (+) or (-) up to 20%, and sometimes up to 10%, of the stated value. It is understood that all numerical designations are preceded by the term "about," even if not explicitly stated. For example, the term "about 10%" should be understood to encompass a range of 9% to 11%, and the term about 100°C indicates a range of 90 to 110°C.

[0191] The present invention will now be illustrated in the following description of experiments carried out in accordance with the present invention. It should be understood that these examples are intended to be illustrative in nature, rather than limiting. Obviously, many modifications and variations of these examples are possible in light of the above teachings. It should therefore be understood that, within the scope of the appended claims, the present invention may be otherwise practiced in a myriad of possible ways than as specifically described below.

[0192] Description of Non-Limiting Examples Example 1 - Processing of household waste into composite materials Apparatus and method In the following examples, various equipment and systems were used. It should be understood that while some of the equipment was adapted for the purposes of the present invention, all were based on conventional equipment. These included shredders, single screw extruders, injection molding machines, compression molding presses, and any other machine in which materials are subjected to shear and / or heat, such as granulators, pelletizing presses, mills, etc.

[0193] in particular, Biodrying (Compost Biodrying System) - Biodrying is activated by bacteria and multicellular organisms present in household waste. This process occurs through the digestion of organic material by bacteria, which produces heat. It is important that household waste is loosely stratified under controlled conditions and ventilated with a precisely defined amount of air. This air must be neither too cold nor too humid, while the blowing force is digitally controlled. Over a period of several days and up to two weeks, municipal waste (MW) heats up, gaining heat up to 70°C. The heat is regulated by a controlled supply of air, setting an optimal process temperature of approximately 55°C to 70°C. When the MW reaches a dryness level of approximately 15-20% moisture, or even 15-18%, bacterial activity decreases significantly, and the biodrying process is considered complete.

[0194] A metal separation magnet (IFE MPQ 900 FP) was used to separate the ferrous materials. The metal separation magnet contains an electromagnet that levitates above the conveyor belt. The coils create a narrow, deep magnetic field that lifts the ferrous metal parts and transports them a short distance through its own conveyor belt, thus separating the magnetic metal from the remaining material. The metal is disposed of in a bin at the bottom of the system and returned to recycling. The magnetic belt system is installed at the end of the conveyor belt, and a box is positioned directly above the flight parabola to capture the magnetic material.

[0195] An eddy current system (Wagner magnet 0429\0-37) was used to separate the metals. Specifically, a 2.5-meter-wide eddy current belt with neodymium high-gradient magnets was used. The pole system was eccentrically mounted inside the slower belt drum. The belt drum had an outer speed of 1 to 3 m / s. The inner drum operated at a maximum of 3,000 rpm. This created an eddy current field that attracted and heated ferrous metals while repelling nonferrous metals (which were therefore removed). The separation force was highest for aluminum and decreased for brass, copper, and other nonferrous metals.

[0196] Eddy current can be replaced with a metal detector to achieve similar results.

[0197] The dry sorted waste was granulated using a shredder (Vecoplan VAZ 1300). Specifically, two types of shredders were used: a primary pre-shredder and a secondary shredder.

[0198] The primary pre-shredder is defined by one, two, three, or four shafts connected to hydraulic or electromechanical drives. The primary pre-shredder is characterized by the high forces generated to break the waste into small pieces. It separates non-friable materials that would otherwise interfere with secondary shredding. The shredding shafts used are mechanically connected to the shaft, and the peripheral speed of the shaft is low.

[0199] Secondary shredding is performed after separation by one or two rotors mechanically connected with abrasive tools and counter blades, and a screen basket is installed in front of the rotors to control particle size.

[0200] An air separation system (IFE UFS600X+1000X) was used to separate the light and heavy particles. Specifically, the air separator / classifier consists of an acceleration belt, on which the particles are arranged in a single layer, and a subsequent air bar, which blows an adjustable, defined air flow into the material. After the air bar, there is usually a separator between the light and heavy particles. Following the separation, there is a dividing space, which gives the light fraction a chance to sink. The heavy material is separated between the air bar and the separator.

[0201] A near-infrared system (SESOTEC MN 1024) was used to selectively separate specific plastic polymers. Specifically, a system with a scanner, active sensor support, and active blow bar was used. In addition, the system was equipped with a high-resolution NIR camera with a sensitivity of at least 1.5 mm, which captures the IR spectral reflection of specific substances and compares it with stored spectra of various substances. If the system detected the desired substance, it queried a freely programmable function in binary format—separate or retain. Then, using the connected blow nozzle bar, the particles were blown off with the same fineness as the detection.

[0202] Selective sorting resulted in a selective heterogeneous waste containing less than 1% PVC and less than 3% PS, and less than 5% PET in particulate form.

[0203] A single-screw extruder (Type F: GRAN 145) was used. Specifically, the extruder had dimensions of 145 mm diameter, 950 cm screw length, 0.5-2 mm screw-to-barrel clearance, high wear resistance screw and barrel, a maximum die opening diameter of 30 mm, and two ventilation zones. During operation, an anti-bridging silo rotor kept the ready-to-use (RTW, i.e., sorted heterogeneous waste) material moving, preventing material bridging and ensuring flowability. The feeder screw was automatically activated depending on the extruder capacity utilization.

[0204] After the extruder process, the material was transferred to a controlled cooling system with an 800 cm long cooling conveyor and an air flow of 15,000 m³ / h.

[0205] Milling Equipment - Several milling equipment was used to reduce the size of the final product, i.e., the composite material.

[0206] Hammer Mill Type 40\32 HA-Hammer mills grind soft to medium hard fragments in a continuous process, the material undergoes a process of particle mixing while grinding, thus creating homogeneity.

[0207] Impact mill (ULTRAPLEX UPZ 500) - Reduced particle size to another level by using high speed rotating blades (beater plates) that "collided" particles between the walls and themselves, and the significant friction between the sides of the grinder (grinding tracks) and the beater plates reduced the material to powder form. The resulting powder was passed through a vibrating sieve system that sieved the particle size by using different size holes with different diameters.

[0208] The reduced particle size was then conveyed from the hammer mill through a blower to the next milling stage, an impact mill.

[0209] Knife Mill (ROTOPLEX 50 / 100) - Particles of 0.9 mm size (and smaller) were stored directly, as were particles of 1.4 mm. Particles of sizes larger than 1.4 mm were further processed using a "Knife Mill" (ROTOPLEX 50 / 100). Specifically, the knife mill is designed to generate high cutting forces at high throughput. Using the "scissors" principle, a drum with knives moves at high speed in front of a counter knife in a cooled environment. Through the knife mill system, particles (especially fibers) were further reduced to sizes smaller than 1.4 mm.

[0210] An elemental analyzer (Flash EA 1112) was used for the determination of total carbon (C), hydrogen (H), nitrogen (N), sulfur (S), and oxygen (O).

[0211] Fourier transform infrared spectroscopy (FTIR) - Nicolet 6700, spectrophotometer for the mid-infrared range. Absorbance spectra were obtained by recording absorbance as a function of wavelength. Concentrations were calculated from absorbance measurements at specific wavelengths based on a publicly known library provided in the manufacturer's operating instructions.

[0212] Thermogravimetry (TG)-Differential Scanning Calorimetry (DSC)-STA TG-DSC 449 F3 Jupiter® (NETZSCH-Geratebau) - The simultaneous application of TG and DSC to a single sample in an STA instrument yields more information than the separate application of TG and DSC in two different instruments. STA allows for simultaneous quantitative monitoring of the mass and thermodynamic changes occurring in a test material under heating. Coupling MS to an instrument for thermal analysis allows for the identification of materials / components released during heating experiments. Thus, the combination of STA TG-DSC with MS provides a unique and simple tool for unambiguous experimental characterization of chemical reactions and phase transformations in a wide range of materials. The TG-DSC was operated under the following conditions:

[0213] [Table 1]

[0214] Gas chromatography-mass spectrometry (GC-MS) - Composite samples were analyzed after 24 hours of headspace extraction using a gas chromatography (GC) sniffer followed by gas chromatography-mass spectrometry (MS). Specifically, an Agilent 7890A GC was equipped with an autosampler, a split / splitless injector, and three detectors: FID, ECD, and TCD. The GC was equipped with electronic control of gas pressure and flow rate.

[0215] Tensile Testing - Tensile properties were determined according to ISO 521-2:1996 using specimen type A1: total length ≥ 150-200 mm, length of narrow parallel-sided portion = 80 ± 2 mm, radius 20-25 mm, distance between wide parallel-sided portions 104-113 mm, width at ends = 20 ± 0.2 mm, width at narrow portion 10 ± 0.2 mm, preferred thickness 4 ± 0.2 mm, gauge length 50 ± 0.5 mm, and initial distance between grips = 115 ± 1 mm.

[0216] Izod Impact (Notched) - Izod impact was measured using ISO 180 (1 J pendulum) / ASTM D256 (1 J pendulum), notched, 1 J hammer. (Izod impact strength, edgewise notched specimens)

[0217] Charpy impact - Charpy impact tests were performed according to ISO 179 using a notched hammer 1 J (Charpy impact strength according to ISO 179, edgewise notched specimen, pendulum weight 1 J).

[0218] Flexural testing - Tests were performed using ASTM D790 (ISO 178) method at a test speed of 5 mm / min.

[0219] Ash content - Ash was determined according to ISO 3451 method A. Two test portions of 5 gr each were used and burned at 950 ± 50°C for 30 minutes.

[0220] Surface Energy - Surface energy was measured using a Dyne Pen per ASTM D2578.

[0221] Oxygen Index - Oxygen Index was determined according to ISO 4589-2.

[0222] Density - Density was measured according to ASTM D792 = ISO1183-1 procedure (Plastics - Methods for determining the density of non-cellular plastics) using an MRC laboratory instrument (model BPS750-C2V2). The specimens should be at least 1 cm3 and at least 1 mm thick (per 1 gr weight).

[0223] method The mixed household waste underwent a pre-sorting and bio-drying process, which began with the removal of metallic particles, ferrous and non-ferrous, using a metal separation magnet (type IFE MPQ 900 FP).

[0224] In the next step, the waste was passed through an eddy current (type Wagner magnet 0429\0-37) pole system installed inside the belt drum. The belt drum had an external speed of 1-3 m / s. The internal drum operated at a maximum of 3000 rpm. This created an eddy current field that repelled non-ferrous metals from the MW flow. At the end of this section, the waste was stripped of metals and transported via conveyor to a bio-drying process (type Compost Systems). The waste at this stage typically contained a high water / humidity content of 30%-50%, and the bio-drying was designed and controlled to reduce the moisture level to less than 20%.

[0225] The biodried MW was then shredded to obtain a waste particle size of (maximum) 30 mm or less. Particles shredded below 30 mm were removed through a dedicated basket, while larger particles continued to rotate in the shredder until they reached the desired size. Notably, shredding created some friction, which further reduced moisture by 2% to 3%. The shredded particles were more uniform, allowing the next stage of the process to work more efficiently.

[0226] Following shredding, some of the impurities "bonded" or encased in the shredded waste particles were released by an air separator system. The shredded material entered an air separator (air classifier (type IFE UFS600X+1000X)) system, which eliminated any associated portion of heavy particles (metals or minerals) from the shredded material (resulting in the formation of a "light fraction").

[0227] The light fraction was then conveyed to a NIR separation system where halogenated polymers such as PVC and aryl-containing synthetic polymers such as polystyrene and / or PET were selectively removed.

[0228] The material after NIR separation provided the sorted heterogeneous incorporation material, which was then subjected to extrusion. The extruder was operated to have an operating temperature of 150°C to 180°C, a residence time of 5 to 7 minutes, and a rotation speed of 60 to 90 rpm.

[0229] After passing through the extruder process, the resulting molten material was cooled to 40°C by a cooling conveyor (length 800 cm, air flow rate 15000 cubic meters / hour).

[0230] The cooled composite material was subjected to size reduction / size refinement by passing it through a hammer mill followed by an impact mill, and then the refined particles were selectively sieved to obtain either a Q0.9 (particles up to 0.9 mm) or a Q1.4 (particles up to 1.4 mm) product.

[0231] Example 2 - Analysis and Characterization DNA extraction and chlorophyll content of Q0.9 and Q1.4 The DNA extraction protocol was adapted from http: / / www.bio-protocol.org / e2906. Specifically, triplicates of 20 g of Q0.9 and Q1.4 were ground to a fine powder in liquid nitrogen using a chilled mortar and pestle (this is a common method for extracting DNA LN2 at -210°C). This fine powder was then placed in a tube, to which 500 μl of 2% chloroform:isoamyl alcohol (24:1) (CTAB) solution was added and incubated in a 65°C water bath for 1 hour with vigorous mixing. The use of CTAB, a cationic surfactant, facilitates the separation of polysaccharides during purification, and additives such as polyvinylpyrrolidone can aid in the removal of polyphenols. CTAB-based extraction buffers are widely used when purifying DNA from plant tissues.

[0232] The mixture was then centrifuged at 12,000 g for 15 minutes, and the supernatant was collected. An equal volume of chloroform was added to the supernatant and centrifuged again. The aqueous phase was collected, and an equal volume of isopropyl alcohol was added by gently mixing the tube. The tube was placed at -20°C for 1 hour and centrifuged at 12,000 x g for 15 minutes. 700 μl of 75% ethanol was added to the pellet, and the mixture was centrifuged at 12,000 x g for 5 minutes. The pellet was completely dried, mixed with 30 μl of ultrapure water and 1 μl of 10% RNase A, and incubated at 37°C for 1 hour. The DNA content was determined using a NanoDrop.

[0233] Chlorophyll content determination was performed using a protocol modified from http: / / www.bio-protocol.org / e2906. Specifically, triplicates of 20 mg of Q were added to 1.5 ml tubes containing 1 ml of dimethylformamide (DMF). The tubes were incubated overnight at 4 °C to allow the chlorophyll to dissolve in the DMF solution. 300 μl of sample solution was mixed with 600 μl of DMF in a new Eppendorf tube (2 volumes of DMF per volume of sample). Absorbance (A) was measured on a spectrophotometer at wavelengths of 647 nm and 664.5 nm using a quartz cuvette. Chlorophyll a content (μg / ml) = (12 × A 664.5 )-(2.79×A 647 ) Chlorophyll b content (μg / ml) = (20.78 × A 647 )-(4.88×A 664.5 )

[0234] [Table 2]

[0235] QElemental analysis of materials (C, H, N) Elemental analysis for C, H, N, S, and O was performed using a Flash EA 1112 elemental analyzer according to the manufacturer's instructions.

[0236] [Table 3]

[0237] ICP-Atomic Emission Spectroscopy The Q0.9 and Q1.4 samples were digested by a microwave digestion system (Milestone Ethos-1) and analyzed by ICP-AES (axial) (Spectro ARCOS-EOP) and ICP-AES (radial) (Spectro ARCOS-SOP) as described above.

[0238] The data obtained is shown in Table 3.

[0239] [Table 4]

[0240] Interestingly, Table 3 shows that both Q0.9 and Q1.4 contain high levels of potassium and magnesium (see also Table 13).

[0241] Fourier transform infrared spectroscopy (FTIR) FTIR spectroscopy was performed using a Nicolet 6700 with the ATR accessory described above.

[0242] FIG. 2 provides results for two different samples, including a 0.9 mm size composite (Q0.9) and a 1.4 mm size composite (Q1.4).

[0243] Interestingly, the FTIR library identified Q0.9 as lutein (86%) and Q1.4 as newsprint (black ink) (92%). While this cannot be considered a definitive chemical identification, it is an interesting observation and a clear distinction between Q0.9 and Q1.4 and from other wood plastics. Q1.4 is relatively rich in cellulose fiber, while Q0.9 contained less fiber and a higher proportion of smaller molecules such as lutein.

[0244] Thermogravimetric Analysis (TGA) - Differential Scanning Calorimetry (DSC) TGA measures weight loss as a function of temperature. A loss of 5% indicates the onset of decomposition. The composite materials disclosed herein were found to be more stable than those disclosed in WO 2010 / 082202 (the contents of which are incorporated herein by reference) (see also Table 13 below). Q0.9 was stable up to 218°C, and Q1.4 was stable up to 224°C. In particular, the higher the onset of decomposition, the wider the processing window.

[0245] The methodology used to analyze the organic / inorganic compounds found in the test samples of Q0.9 and Q1.4 was based on thermal analysis techniques as follows: a. Differential scanning calorimeter (DSC) to determine the relative amounts of synthetic polymers. b. Thermal stability (T 開始 and T0), the amount of inorganic material (ash content), and thermogravimetric analysis (TGA) to determine the approximate amount of lignocellulosic components.

[0246] result Lignocellulose content - approximately 350°C (from TGA) Inorganic content - ash>650℃ (from TGA)

[0247] The coupling of MS to instruments for thermal analysis allows the identification of materials / components released during heating experiments.

[0248] Table 4 and Figures 1A-1B provide the thermal stability of the composite materials disclosed herein, namely Q0.9 and Q1.4.

[0249] [Table 5]

[0250] Figure 1A shows the TG-DSC of Q1.4 from 0 to 1500 °C with an increment of 50 °C per minute.

[0251] Figure 1B shows the TG-DSC of Q0.9 from 0 to 1500 °C with a 50 °C increase per minute.

[0252] As can be seen, the TGA peaks in each of the graphs correspond to T 開始 The graphs show the mass evolution with the onset of the decrease at T and the maximum decrease at T, while the DSC graph shows the resulting energy release. These two figures show that the complex is stable at temperatures above 210°C.

[0253] The composition of each sample, Q0.9 and Q1.4, was also determined by combined MS and the data are shown in Table 5.

[0254] [Table 6]

[0255] Total Extractable Carbon Total extracted carbon was determined using 20 g of Q0.9 and Q1.4 extracted with dimethyl ether (DME). The oil residue was weighed and the amount of extracted carbon was calculated. The results are shown in Table 6.

[0256] [Table 7]

[0257] It is noteworthy that both Q0.9 and Q1.4 contained significant amounts of extracted carbon. DME decomposes in organic solvents. Therefore, it is assumed that the majority of the carbon content is derived from fatty acids. This is also confirmed by GC-MS below.

[0258] Tensile test Tensile test specimens were prepared as follows: The composite material was extruded at 170-180°C and 350 rpm using a ZSK 18 laboratory extruder to obtain a homogeneous material. The extrudate was then pulverized using a laboratory granulator, and the granular material was injection molded at 170-180°C using a Haitian 120T to produce test specimens. Test specimens were then conditioned at 23±2°C for at least 48 hours.

[0259] Measurement of tensile properties of injection molded samples was provided using ISO 521-2:1996.

[0260] Specimen type 1A included the following dimensions: total length ≥ 150-200 mm, length of narrow parallel-sided portion = 80 ± 2 mm, radius 20-25 mm, distance between wide parallel-sided portions 104-113 mm, width at end = 20 ± 0.2 mm, width at narrow portion 10 ± 0.2 mm, preferred thickness 4 ± 0.2 mm, gauge length 50 ± 0.5 mm, and initial distance between grips = 115 ± 1 mm.

[0261] At least five specimens were tested on a Tinius Olsen H10KT instrument at a test speed of 50 mm / min. The test results are the average of these measurements.

[0262] Table 7 provides a summary of the physical properties.

[0263] [Table 8]

[0264] Impact Izod (notched) The notched Izod impact is a single-point test that measures a material's resistance to impact from a pendulum. The Izod impact (notched) is defined as the kinetic energy required to initiate and continue failure until the specimen breaks.

[0265] At least five specimens were tested with a Tinus Olsen impactor, model 503 (pendulum weight 1 J). The test results, which are the average of these measurements, are shown in Table 8.

[0266] [Table 9] * N-Non / P-Partial / C-Complete / H-Hinge

[0267] Q0.9 and Q1.4 showed improved Izod impact compared to the composites of WO 2010 / 082202 (see also Table 13).

[0268] Charpy impact The Charpy impact test is a single-point test that measures the resistance of a material to impact from a pendulum. The Charpy impact is defined as the kinetic energy required to initiate and sustain fracture until the specimen breaks. The resulting value can be used for quality control or to distinguish between general toughness.

[0269] At least five specimens were tested with a Tinus Olsen impactor, model 503 (pendulum weight 1 J). The results presented in the table are the average of these measurements.

[0270] Table 9 shows the Charpy impacts for Q0.9 and Q1.4.

[0271] [Table 10] * N-Non / P-Partial / C-Complete / H-Hinge

[0272] Q0.9 and Q1.4 showed improved Charpy impact compared to the composites of WO 2010 / 082202 (see also Table 12).

[0273] Bending test The flexural test measures the force required to bend a beam under a three-point load condition. The data is often used to select materials for components that will support the load without deflection. The flexural modulus is used as an indication of the stiffness of a material when bent.

[0274] At least five specimens were tested on a Tinius Olsen H10KT instrument, and the results presented in Table 10 are the average of these measurements.

[0275] [Table 11]

[0276] ash An ash test was used to determine whether Q0.9 or Q1.4 was filled. The test typically identifies the total filler content or inorganic content. Test samples were 5 g each.

[0277] The ash results for Q0.9 and Q1.4 are 10.4% and 7.9%, respectively.

[0278] It should be noted that low ash content means less mineral in the composite, resulting in better thermoplastic properties. It is clear that compared to the composites of WO 2010 / 082202, the composites disclosed herein have significantly lower ash content.

[0279] Surface Energy The strength of the attraction between a material and a coating is determined by the relative surface energy / surface tension of the materials. The higher the surface energy of the solid relative to the surface tension of the liquid, the greater the molecular attraction, which draws the paint, ink, or adhesive closer together, resulting in a stronger bond. The lower the surface energy of the solid relative to the surface tension of the liquid, the weaker the attraction, which repels the coating.

[0280] The surface energies of Q0.9 and Q1.4 were found to be identical, 36 dynes / cm. Regarding surface energy, it should be noted that most solvent-based printing requires plastics to be treated to 36-40 dynes / cm. Therefore, Q0.9 and Q1.4 exhibit very good surface energies, unlike typical plastics.

[0281] Oxygen Index To measure combustion behavior by oxygen index, a test specimen is supported vertically in a mixture of oxygen and nitrogen flowing upward through a transparent chimney. The top end of the specimen is ignited, and the subsequent burning behavior of the specimen is observed. The duration of burning, or the length of the specimen that has burned, is compared with the specified limit for such burning. By testing a series of specimens at different oxygen concentrations, the minimum oxygen concentration is estimated.

[0282] Based on the above, the oxygen index of Q0.9 was 21.3%.

[0283] density Density is kg / m 3 The density is the ratio of the mass of the sample to the volume of the sample, expressed as 1 cm. To determine the density, the samples were conditioned at 23°C ± 2°C and 50 ± 5% room humidity for 40 hours. The volume of the specimen is 1 cm. 3 The specimens were at least 1 mm thick for each 1 g weight, and the surfaces and edges were smooth. Specimens weighing 1 to 5 g have been found to be convenient, although specimens weighing approximately up to 50 g are also acceptable.

[0284] For density determination, the specimen is weighed in air (A) and then weighed again in a supplementary liquid (B) of known density, in this example ethanol.

[0285] The density ρ of the solid is then calculated according to the following formula:

[0286]

number

[0287] The density of ethanol is 789 kg / m 3 and the density of air is 1.225 kg / m 3 is.

[0288] Density is determined at standard room temperature of 23°C ± 2°C.

[0289] The densities of Q1.9 and Q1.4 at 23°C relative to ethanol are shown in Table 11.

[0290] [Table 12]

[0291] Since plastics are sold on a cost-per-pound basis, and lower density (or lower specific gravity) means more material per unit of weight, it is desirable to have a low-density product. As shown in Table 13, the densities of Q0.9 and Q1.4 were lower than the composites described in WO 2010 / 082202.

[0292] Example 3 - Comparison with composite material from WO 2010 / 082202 To assess the superiority of the composite materials disclosed herein, a comparison was made with the composite materials disclosed in WO 2010 / 082202. Table 12 provides the comparison.

[0293] [Table 13] + - indicates that the element is found to be present. ND-indicates that the element was not detected.

Claims

1. A composite material comprising: a. at least 40% w / w of a total weight of the composite material of non-plastic organic material, the non-plastic organic material comprising at least cellulose; b. 10% to 60% by weight of the total weight of the composite material of a synthetic plastic material, the synthetic plastic material comprising a plurality of synthetic thermoplastic polymers; c. A homogeneous blend of a heterogeneous combination of synthetic plastic, non-plastic organic, and inorganic materials, including up to 15% w / w inorganic materials; the composite material comprises an aryl-containing synthetic polymer in an amount of less than 10% w / w of the total weight of the composite material and a halogenated polymer in an amount of less than 1% w / w of the total weight of the composite material; the plastic material comprises more than two polyolefins and more than two non-polyolefins; The composite material has the following properties: - the composite has a notched Izod impact of at least 15 J / m, and - the sample of said composite material subjected to injection moulding a tensile strength of at least 8 MPa, and a flexural strength of at least 15 MPa.

2. 10. The composite material of claim 1, comprising PET in an amount less than 5% of the total weight of the composite material.

3. Features include: the composite material has a density of 1.2 gr / cm ３ having a density of: - the composite material has a thermogravimetric analysis (TGA) temperature greater than 200°C; - the sample of said composite material subjected to injection moulding a tensile strength of at least 10 MPa, a tensile modulus of at least 1,500 MPa, a flexural modulus of at least 1,500 MPa, and a bending strength of at least 20 MPa, and - the composite material contains less than 5 mg / g of silicates.

4. 1.2 gr / cm ３ 4. The composite material according to claim 1, having a density of:

5. 5. The composite material of any one of claims 1 to 4, having a thermogravimetric analysis (TGA) temperature above 200°C.

6. In a sample of the composite material subjected to injection molding, the sample - a tensile strength of at least 10 MPa, a tensile modulus of at least 1,500 MPa, a flexural modulus of at least 1,500 MPa, and A composite material according to any one of claims 1 to 5, having a flexural strength of at least 20 MPa.

7. 7. The composite material of any one of claims 1 to 6, comprising less than 5 mg / g silicate.

8. 8. A composite material according to any one of claims 1 to 7 in the form of micronised particles having a size distribution of d90 of less than or equal to 1,500 μm as measured by sieving through a 1,500 μm sieve.

9. 9. A composite material according to any one of claims 1 to 8 in the form of micronised particles having a size distribution of d90 equal to or less than 900 μm as measured by sieving through a 900 μm sieve.

10. 1. A method for preparing a composite material, said method comprising: a. subjecting a particulate heterogeneous incorporation material to at least one extrusion process in an extruder at a temperature maintained within the range of 150°C and 200°C, thereby obtaining said composite material; The particulate foreign incorporation material is i. at least 40% w / w of non-plastic organic matter by total weight of heterogeneous waste, the non-plastic organic matter comprising at least cellulose; ii. 10% w / w to 60% w / w of the total weight of the composite material of a synthetic plastic material comprising a plurality of synthetic thermoplastic polymers, the synthetic plastic material comprising more than two polyolefins and more than two non-polyolefins; iii. up to 15% w / w of inorganic material of the total weight of the composite material; The method of claim 1, wherein the heterogeneous incorporation material comprises a heterogeneous combination of synthetic plastic, non-plastic, and inorganic materials, and the heterogeneous incorporation material comprises an aryl-containing synthetic polymer in an amount of less than 10% w / w of the total weight of the composite material and a halogenated polymer in an amount of less than 1% w / w of the total weight of the composite material.

11. The method of claim 10 , wherein the aryl-containing synthetic polymer comprises PET.

12. 12. The method of claim 11, wherein the entrapment material comprises PET in an amount less than 5% w / w of the total weight of the composite material.

13. 13. The method of any one of claims 10 to 12, comprising subjecting the particulate heterogeneous waste to at least one separation step prior to the extrusion process, the separation step comprising removing one or both of halogenated polymers and aryl synthetic polymers from the particulate heterogeneous waste based on near infrared (NIR) absorbance to obtain sorted heterogeneous waste.

14. 14. The method according to any one of claims 10 to 13, wherein the particulate heterogeneous entrapment material is obtained by subjecting heterogeneous waste to two or more granulation and sieving steps.

15. A method according to any one of claims 10 to 14, comprising controlled slow cooling of the extrudate discharged from the extruder.

16. A method according to any one of claims 10 to 15, wherein the composite material is subjected to at least one micronization step comprising a size reduction of the composite material.

17. 17. The method of claim 16, wherein the size reduction is to a size defined by a d90 of 1,500 mm or less.

18. An article of manufacture comprising a homogeneous blend of the composite material of any one of claims 1 to 9 and at least one polyolefin.

19. 10. A method of producing an article of manufacture, said method comprising processing the composite material of any one of claims 1 to 9 with at least one polyolefin, said processing comprising at least one of extrusion and molding, said processing providing an intimate blend of said composite material with said at least one polyolefin.

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