Mixture of materials with improved performance and methods of manufacture and use of the same

Description

1 / 53 A blend of materials with improved performance and methods of manufacturing and using them. CROSS-REFERENCE TO RELATED REQUESTS

[001] This application is an international PCT application of a US Continuation-in-Part Application No. 18 / 170,450 filed February 16, 2023, which claims the benefit of and priority to US Patent Application No. 17 / 590,466, filed January 1, 2022, and claims the benefit of and priority to US Patent Application No. 63 / 145,174, filed February 3, 2021, and US Provisional Application No. 63 / 282,514, filed November 23, 2021, all of which are incorporated herein by reference in their entirety. FIELD OF THE INVENTION

[002] The present invention relates to a mixture of materials with improved performance when applied to a substrate. The present invention relates to a composite product using a mixture of materials. FUNDAMENTALS OF THE INVENTION

[003] Melamine-Urea-Formaldehyde (MUF) resins have become popular for use as adhesives in particleboard (PB) or medium-density fiberboard (MDF) because they have been found to reliably improve physical properties such as internal bond strength (IB), modulus of rupture (MOR), modulus of elasticity (MOE), and water resistance properties, as measured by water absorption (WA) and thickness swelling (TS), compared to urea-formaldehyde (UF) resins. Urea-formaldehyde resins are well known in the art for the same applications; however, these resins have been found to produce relatively weaker particleboard and medium-density fiberboard with unsatisfactory water resistance properties, as evidenced by the graph in Figure 10. Figure 10 shows the difference in internal bond strength. Petition 870260076067, dated 07 / 30 / 2026, page 7 / 62 2 / 53 between UF resins and MUF resins in the equivalent molar ratio of F to U and F to M + U (hereinafter, the RM ratio), respectively with increased panel groups.

[004] Although MUF resins provide these enhanced characteristics, there is a need for an alternative to melamine that is more environmentally friendly while maintaining the same resin performance.

[005] WO 2016 / 057390 (WO '390) refers to adhesives containing from about 20% by weight to about 40% by weight of an aldehyde-based resin, from 1% by weight to about 15% by weight of a kraft lignin, from 0.05% by weight to about 2% by weight of a surfactant, and from 0.5% by weight to about 10% by weight of an alkaline compound, and methods for manufacturing and using the same. WO '390 adhesives may have a viscosity of from about 500 cP to about 5,000 cP at a temperature of about 250°C.

[006] US 8,252,864 (US '864) refers to a curable urea / formaldehyde resin composition and a reconstituted wood product made by combining curable urea / formaldehyde resin with a particulate lignocellulosic material.

[007] There is still a need to modify amino resins to improve adhesive performance characteristics while reducing the environmental impact by consuming byproducts from other industrial processes. SUMMARY OF THE INVENTION

[008] In some embodiments, a mixture of materials may include a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin; a lignosulfonate or a kraft lignin; an alkaline compound; optionally an additive; and a plurality of substrates, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

[009] In other forms, a method for preparing a Petition 870260076067, dated 07 / 30 / 2026, page 8 / 62 3 / 53 The mixture of materials may include adding a plurality of substrates; mixing a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin optionally with an amine and water to a pH of 5-11, preferably 6-10; optionally adding one or more additives; adding a lignosulfonate salt or a kraft lignin; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

[0010] In certain embodiments, a method for preparing a mixture of materials may include adding a plurality of substrates; mixing a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin, a lignosulfonate salt or a kraft lignin optionally with an amine and water to a pH of 5-11, preferably 6-10; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

[0011] In some embodiments, a method for preparing a mixture of materials may include adding a plurality of substrates; mixing a lignosulfonate salt or kraft lignin with the substrates; adding a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin, optionally with an amine and water at a pH of 5-11, preferably 6-10; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 hours. Petition 870260076067, dated 07 / 30 / 2026, page 9 / 62 4 / 53 days.

[0012] In additional embodiments, a composite product may include a plurality of substrates; and a mixture of materials that is at least partially cured, wherein the mixture of materials, prior to curing, may include a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin; a lignosulfonate or a kraft lignin; an alkaline compound; and optionally, one or more additives; wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

[0013] In order to meet this need, the present disclosure relates to a resin system and methods of manufacturing the resin system in which lignosulfonate is added to UF and MUF adhesives. One aspect of the present invention is based on the addition of lignosulfonate to amino resins which enhances the adhesive performance characteristics while reducing the environmental impact by consuming byproducts from other industrial processes.

[0014] In a first aspect, the disclosure refers to a resin system comprising: a urea-formaldehyde (UF) or melamine-urea-formaldehyde (MUF) resin, prepared by: Mix one or more urea compounds, one or more formaldehyde compounds, a buffering and stabilizing agent, and optionally one or more melamine compounds to form a mixture, optionally heating while mixing for at least one minute, to form a UF resin or a MUF resin, wherein the UF resin or the MUF resin has a molar ratio (MR) of total moles of formaldehyde to total moles of urea plus, if present, one or more melamine compounds of about 0.25:1 to about 2.50:1, or of about 0.25:1 to about 1.5:1, and if the pH of the UF resin or the MUF resin is not 6.5 Petition 870260076067, dated 07 / 30 / 2026, p. 10 / 62 5 / 53 to about 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0, then one or more alkaline compounds or acidic compounds are mixed with the UF resin or MUF resin until the pH is 6.5 to about 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0 to form the resin system, wherein one or more lignosulfonate compounds are added to the mixture or are added to the UF resin or MUF resin formed in an amount of about 0.1% by weight to about 30% by weight, or from about 1.0% by weight to about 20% by weight, or from about 1.0% by weight to about 10% by weight, based on a total weight of the resin system, about 0.0% by weight to about 40% by weight of water, based on the total weight of the resin system, and wherein the resin system has a buffer capacity of 2 to 400 mL, or greater than 5 to 150 mL, preferably 20 to 60 mL of 0.1 N HCl by the ATV method for a period of at least about 20 days at 25°C.

[0015] In the above embodiment, urea-formaldehyde (UF) or melamine-urea-formaldehyde (MUF) resins can be prepared by: Mix a first set of components comprising one or more urea compounds and one or more formaldehyde compounds and, optionally, one or more melamine compounds, optionally heating while mixing for at least one minute, to form a first reaction product having an initial molar ratio (IMR) of total moles of one or more formaldehyde compounds to moles of one or more urea compounds plus, if present, one or more melamine compounds of about 0.7:1 to 7:1, or about 1:1 to 5:1, or 1.4:1 to 4.5:1 until complete condensation; mix the first reaction product with a second set of components comprising one or more compounds of Petition 870260076067, dated 07 / 30 / 2026, p. 11 / 62 6 / 53 Urea and a buffering and stabilizing agent and, optionally, one or more melamine compounds, optionally heated while mixing to form UF resin or MUF resin, wherein the UF resin or MUF resin may have a molar ratio (MR) of total moles of formaldehyde to total moles of urea plus, if present, one or more melamine compounds of about 0.25:1 to about 2.50:1, or of about 0.25:1 to about 1.5:1, and if a pH of the UF resin or MUF resin is not from 6.5 to about 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0, then one or more alkaline compounds or acidic compounds may be mixed with the UF resin or MUF resin until the pH is 6.5 to about 9.0. 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0 to form the resin system,wherein one or more lignosulfonate compounds may be included with the first set of components and / or with the second set of components and / or after the formation of the UF resin or MUF resin in an amount of about 0.1% by weight to about 30% by weight, or about 1.0% by weight to about 20% by weight, or about 1.0% by weight to about 10% by weight, based on a total weight of the resin system, about 0.0% by weight to about 40% by weight of water, based on the total weight of the resin system, and wherein the resin system may have a buffer capacity of 2 to 400 mL, or greater than 5 to 150 mL, preferably 20 to 60 mL of 0.1 N HCl by the ATV method for a period of time of at least about 20 days at 25°C. This second step of mixing the first reaction product with a second set of components comprising one or more urea compounds and a buffering and stabilizing agent may be carried out for any number of reasons.One of which may be to retain any excess formaldehyde remaining from the first step. The inventive resin system can be prepared in one step, Petition 870260076067, dated 07 / 30 / 2026, page 12 / 62 7 / 53 two stages, three stages or more.

[0016] In each of the preceding embodiments, one or more melamine compounds may be added, or melamine compounds may be excluded, or Kraft lignin may be excluded.

[0017] In each of the preceding embodiments, one or more melamine compounds may be added in a molar ratio of up to 1:1 with the total moles of one or more urea compounds in the resin system, or one or more melamine compounds may be added in a molar ratio of 0.001:1 to 0.5:1 with the total moles of one or more urea compounds in the resin system, or one or more melamine compounds may be added in a molar ratio of 0.01:1 to 0.25:1 with the total moles of one or more urea compounds in the resin system.

[0018] In each of the preceding embodiments, the resin system comprising one or more lignosulfonates may have a color that is noticeably different from the color of pure UF / MUF resins; or wherein, within 72 hours of resin system formation, 1 liter of the resin system may have an orange, yellow, red, beige, or brown color; or wherein, within 72 hours of resin system formation, the resin system may have a color that is in the range of 4 to 40+ using the official AIH SRM (Standard Research Method) numerical scale for beer color. Alternatively, the resin system is in a range of 19 to 36, or 20 to 35 using the official AIH SRM (Standard Research Method) numerical scale.

[0019] In each of the preceding embodiments, the resin system may include from about 5% by weight to about 40% by weight, or from about 10% by weight to about 35% by weight, or from about 15% by weight to about 30% by weight of one or more formaldehyde compounds, from about 5% by weight to about 35% by weight, or from about 10% by weight to about 30% by weight or from about 15% Petition 870260076067, dated 07 / 30 / 2026, p. 13 / 62 8 / 53 by weight to about 25% by weight of one or more urea compounds in the first set of components, about 5% by weight to about 50% by weight, or about 10% by weight to about 45% by weight, or about 15% by weight to about 40% by weight of one or more urea compounds in the second set of components, about 0.1% by weight to about 30% by weight, or about 0.1% by weight to about 25% by weight, or about 0.1% by weight to about 20% by weight, or about 1.0% by weight to about 15% by weight, or about 2.0% by weight to about 5.0% by weight, or more than 2.0% by weight to about 5.0% by weight of lignosulfonate, about 0.0% by weight to about 40% by weight of water, and where each percentage by weight is based on the total weight of the resin system.

[0020] In each of the preceding embodiments, the pH of the resin system, which is from more than 6.5 to about 10.0, or from about 8.0 to about 9.0, may be due to the effect of the buffering and stabilizing agent, and there is no need to add one or more alkaline compounds or acidic compounds. In each of the preceding embodiments, the resin systems may include melamine in an amount of about 0.0% by weight to about 30% by weight, or from about 0.0% by weight to about 25% by weight, or from about 0.0% by weight to about 20% by weight, or from about 0.1% by weight to about 15% by weight, based on the total weight of the resin system. In some embodiments, no melamine is added to the resin composition.

[0021] In each of the preceding embodiments, the lignin species may be selected from calcium lignosulfonate, magnesium lignosulfonate, ammonium lignosulfonate, or sodium lignosulfonate, preferably ammonium lignosulfonate or sodium lignosulfonate. Petition 870260076067, dated 07 / 30 / 2026, page 14 / 62 9 / 53

[0022] In each of the preceding embodiments, the UF or MUF resin, excluding the lignin species, may have a number-average molecular weight (Mn) of about 300 daltons to about 20,000 daltons, or about 1,000 daltons to about 10,000 daltons, or about 1,500 daltons to about 9,000 daltons, or about 2,000 daltons to about 5,000 daltons; the weight-average molecular weight (Mw) is about 1,000 to about 400,000, or about 30,000 to about 200,000 daltons, as measured by gel permeation chromatography; and the polydispersity (Mw / Mn) is about 10-100.

[0023] In each of the preceding embodiments, the alkaline compound may be selected from a Group I or II metal hydroxide, preferably the alkaline compound is sodium hydroxide, potassium hydroxide, ammonium hydroxide, or any mixture thereof.

[0024] In each of the preceding embodiments, the resin system is stable and may have a kinematic viscosity of about 100 to about 1,500 cSt, or about 100 to about 1,000 cSt, or about 100 to about 600 cSt at a temperature of about 250°C, as measured by the GardnerHoldt viscosity method, for a period of time of at least about 20 days at 250°C, wherein the period of time begins when the resin system is initially produced, and the resin system may have a fast cure rate so as to achieve an improvement in internal bond strength when compared to the control resin system of up to 20%, preferably 10% to 20% at < 7.0 press factor at a plate temperature of 350°F (176.6°C). When measured at full cure with a press factor < 7.0 at a plate temperature of 350°F (176.6°C), the internal bond strength (IB) is at least as good for the inventive resin as compared with the comparator resin. The control resin is the UF resin from Comparator Example B, below.

[0025] In a second aspect, the revelation refers to a Petition 870260076067, dated 07 / 30 / 2026, page 15 / 62 10 / 53 adhesive, including the resin system of each of the preceding embodiments.

[0026] In a third aspect, the revelation refers to a mixture of materials, including a plurality of granular or fibrous lignocellulose substrates and the adhesive of the above embodiment.

[0027] In a fourth aspect, the disclosure relates to a lignocellulosic composite product, including a plurality of lignocellulosic substrates and a resin system that is at least partially cured, wherein the resin system, before curing, includes each of the preceding embodiments of the resin system.

[0028] In the above embodiment, the composite product may be a particleboard, a fiberboard, a plywood, an oriented strand board, or a laminated veneer panel, medium density fiberboard, most preferably, the composite product is a particleboard or medium density fiberboard.

[0029] In a fifth aspect, the disclosure relates to a composite comprising: the inventive resin system of each of the preceding embodiments and a glass mat or abrasives, or the inventive resin system of each of the preceding embodiments in a glass fiber nonwoven, or the inventive resin system of each of the preceding embodiments as an impregnation resin in one or more layers of an overlay.

[0030] In the preceding embodiment, the composite may be a nonwoven fiberglass fabric.

[0031] In each of the preceding embodiments, the glass fiber nonwoven can have an average fiber length of 0.75-2.5 inches (19.05-63.5 mm), preferably 1.0-1.6 inches (25.4-40.64 mm). The resin system containing the glass fibers can be cured at 200-250°C for up to one minute. Petition 870260076067, dated 07 / 30 / 2026, page 16 / 62 11 / 53 Preferably, the resin system containing the glass fibers can be cured at 230°C for 15 seconds. Also, the average base weight of the resin in the composite can be 1.4 - 2.0 lbs / 100 square feet (0.0683 - 0.0976 kg / m2). Preferably, the average base weight of the resin in the composite can be 1.5 - 1.75 lbs / 100 square feet (0.0732 - 0.0854 kg / m2). Furthermore, the average loss on ignition can be 15-30%. Preferably, the average loss on ignition can be 18-25%.

[0032] In each of the preceding embodiments, the glass fiber nonwoven fabric manufactured from the inventive resin system, comprising one or more lignosulfonate compounds, may have a tensile strength in the dry state greater than 10%, preferably greater than 15% to 35%, more preferably greater than 25% to 30% when compared with essentially the same glass fiber nonwoven fabric manufactured from the same resin system except without the one or more lignosulfonate compounds. The tensile strength in the dry state of the glass fiber nonwoven products may be tested on a Thwing-Albert tensile tester (150 kg load cell).

[0033] In a sixth aspect, the disclosure relates to a method for manufacturing a resin system, comprising: mixing one or more urea compounds, one or more formaldehyde compounds, a buffering and stabilizing agent and, optionally, one or more melamine compounds to form a mixture, optionally heating while mixing for at least one minute, to form a UF resin or a MUF resin, wherein the UF resin or the MUF resin has a molar ratio (MR) of total moles of formaldehyde to total moles of urea plus, if present, one or more melamine compounds of about 0.25:1 to about 2.50:1, or of about 0.25:1 to about 1.5:1, and if a pH of the UF resin or the MUF resin is not 6.5 to about 10.0, or of about 8.0 to about 10.0, or of about Petition 870260076067, dated 07 / 30 / 2026, p. 17 / 62 12 / 53 from 8.0 to about 9.0, then one or more alkaline compounds or acidic compounds are mixed with the UF resin or the MUF resin until the pH is 6.5 to about 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0 to form the resin system, wherein one or more lignosulfonate compounds are added to the mixture or are added to the UF resin or resin. MUF formed in an amount of about 0.1% by weight to about 30% by weight, or about 1.0% by weight to about 20% by weight, or about 1.0% by weight to about 10% by weight, based on a total weight of the resin system, about 0.0% by weight to about 40% by weight of water, based on the total weight of the resin system, and wherein the resin system has a buffer capacity of 2 to 400 mL, or greater than 5 to 150 mL, preferably 20 to mL of 0.1 N HCl by the ATV method for a period of time of at least about 20 days at 25°C.

[0034] In the embodiment above, the method for manufacturing a resin system may comprise: Mix a first set of components comprising one or more urea compounds, and one or more formaldehyde compounds and, optionally, one or more melamine compounds, optionally heating while mixing for at least one minute, to form a first reaction product having an initial molar ratio (IMR) of total moles of the one or more formaldehyde compounds to moles of the one or more urea compounds plus, if present, the one or more melamine compounds of about 1.4:1 to 5:1, or about 1.4:1 to 3:1, or about 2; mix the first reaction product with a second set of components comprising one or more urea compounds and a buffering and stabilizing agent and, optionally, one or more melamine compounds and, optionally, heating while mixing to form a UF resin or a MUF resin, wherein Petition 870260076067, dated 07 / 30 / 2026, p. 18 / 62 13 / 53 If the UF resin or MUF resin has a molar ratio (MR) of total moles of formaldehyde to total moles of urea plus, if present, one or more melamine compounds of about 0.25:1 to about 2.50:1, or about 0.25:1 to about 1.5:1, and if the pH of the UF resin or MUF resin is not from 6.5 to about 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0, then one or more alkaline compounds or acidic compounds may be mixed with the UF resin or MUF resin until the pH of the UF resin or MUF resin is greater than 8.0 or at least 8.4, or is 6.5 to about 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0 are obtained to form the resin system, in which one or more lignosulfonate compounds are included with the first set of components and / or with the second set of components in an amount of about 0.1% by weight to about 30% by weight, or from about 1.0% by weight to about 20% by weight, or from about 1.0% by weight to about 10% by weight, based on a total weight of the resin system, about 0.0% by weight to about 40% by weight of water, based on the total weight of the resin system, and wherein the resin system has a buffer capacity of 2 to 400 mL, or greater than 5 to 150 mL, preferably 20 to mL of 0.1 N HCl by the ATV method for a period of time of at least about 20 days at 25°C.

[0035] In each of the preceding embodiments of the method, melamine may be added, melamine may be omitted, or kraft lignin may be omitted.

[0036] In each of the preceding embodiments of the method, one or more melamine compounds may be added in up to a 1:1 molar ratio with the total moles of one or more urea compounds in the resin system, or one or more melamine compounds may be added in a molar ratio of 0.001:1 to 0.5:1 with the total moles of one or more urea compounds in the system. Petition 870260076067, dated 07 / 30 / 2026, page 19 / 62 14 / 53 of resin, or one or more melamine compounds may be added in a molar ratio of 0.01:1 to 0.25:1 with the total moles of one or more urea compounds in the resin system.

[0037] In each of the preceding embodiments of the method, the resin system comprising one or more lignosulfonates may have a color that is visibly different from the color of resins. Pure UF / MUF; or wherein, within 72 hours of resin system formation, 1 liter of the resin system may have an orange, yellow, red, beige, or brown color; or wherein, within 72 hours of resin system formation, the resin system may have a color that is in the range of 4 to 40+ using the official AIH SRM (Standard Research Method) numerical scale for beer color.

[0038] In each of the preceding embodiments of the method, the resin system may include about 5% by weight to about 40% by weight, or about 10% by weight to about 35% by weight, or about 15% by weight to about 30% by weight of one or more formaldehyde compounds, about 5% by weight to about 35% by weight, or about 10% by weight to about 30% by weight, or about 15% by weight to about 25% by weight of one or more urea compounds in the first set of components, about 5% by weight to about 50% by weight, or about 10% by weight to about 45% by weight, or about 15% by weight to about 40% by weight of one or more urea compounds in the second set of components, about 0.1% by weight to about 30% by weight weight, or from about 0.1% by weight to about 25% by weight, or from about 0.1% by weight to about 20% by weight, or from about 1.0% by weight to about 15% by weight, or from about 2.0% by weight to about 5.0% by weight, or more than 2.0% by weight to about 5,0% by weight of lignosulfonate, Petition 870260076067, dated 07 / 30 / 2026, page 20 / 62 15 / 53 approximately 0.0% by weight to approximately 40% by weight of water, wherein each percentage by weight is based on the total weight of the resin system.

[0039] In each of the preceding embodiments of the method, the pH of the resin system is greater than 6.5 to about 10.0, or from about 8.0 to about 9.0 due to the effect of the buffering and stabilizing agent and there is no need to add one or more alkaline compounds or acidic compounds.

[0040] In each of the preceding embodiments of the method, melamine may be present in an amount of about 0.0% by weight to about 30% by weight or about 0.0% by weight to about 25% by weight, or about 0.0% by weight to about 20% by weight or about 0.1% by weight to about 15% by weight, based on the total weight of the resin system. In some embodiments, no melamine is added to the resin composition.

[0041] In each of the preceding embodiments of the method, the lignin species may be selected from calcium lignosulfonate, magnesium lignosulfonate, ammonium lignosulfonate, or sodium lignosulfonate, preferably ammonium lignosulfonate or sodium lignosulfonate.

[0042] In each of the preceding embodiments of the method, the UF resin or the MUF resin, excluding the lignin species, may have a number-average molecular weight (Mn) of about 300 daltons to about 20,000 daltons, or from about 1,000 daltons to 10,000 daltons, or from about 1,500 daltons to about 9,000 daltons, or from about 2,000 daltons to about 5,000 daltons; the weight-average molecular weight (Mw) is about 1,000 to about 400,000, or from about 30,000 to about 200,000 daltons; and the polydispersity (Mw / Mn) is about 10-100.

[0043] In each of the preceding modalities of the method, Petition 870260076067, dated 07 / 30 / 2026, page 21 / 62 16 / 53 The alkaline compound may be selected from a Group I or II metal hydroxide, preferably the alkaline compound may be selected from sodium hydroxide, potassium hydroxide, ammonium hydroxide, or any mixture thereof.

[0044] In each of the preceding embodiments of the method, the acidic compound may be selected from chloric acid, hydrobromic acid, hydrochloric acid, hydroiodic acid, nitric acid, perchloric acid, sulfuric acid, sulfurous acid, phosphoric acid, acetic acid, formic acid, benzoic acid, oxalic acid, hydrogen sulfate ion, nitrous acid, hydrofluoric acid, carbonic acid, methanoic acid, or any mixtures thereof.

[0045] In each of the preceding embodiments, the resin system is stable and may have a kinematic viscosity of about 100 to about 1500 cSt, or about 100 to about 1000 cSt, or about 100 to about 600 cSt at a temperature of about 250°C, as measured by the GardnerHoldt viscosity method, for a period of at least about 20 days at 250°C, wherein the period of time begins when the resin system is initially produced, and the resin system may have a rapid cure rate so as to achieve an improvement in internal bond strength when compared to the control resin system of up to 20%, preferably 10% to 20% at < 7.0 press factor at a plate temperature of 350°F (176.6°C), when measured at full cure at < 7.0 press factor at a plate temperature of At 350°F (176.6°C), the internal bond strength (IB) is at least as good for the inventive resin as compared with the comparator resin.The control resin is Comparative Example B, discussed below.

[0046] Additional details and advantages of revelation will be specified in part in the following description and / or can be learned through the practice of revelation. The details and advantages of revelation can be obtained and achieved through the elements Petition 870260076067, dated 07 / 30 / 2026, page 22 / 62 17 / 53 and combinations specifically indicated in the attached claims. It should be understood that both the previous general description and the detailed description below are merely exemplary and explanatory and are not restrictive of the disclosure, as claimed. BRIEF DESCRIPTION OF THE DRAWINGS

[0047] Figure 1 shows the viscosity stability over time for Comparative Examples A and B and Inventive Examples 1-3 at 25°C.

[0048] Figure 2 shows the viscosity stability over time for Comparative Examples A and B and Inventive Examples 1-3 at 35°C.

[0049] Figure 3 shows the pH decay over time for Comparative Examples A and B and Inventive Examples 1-3 at 25°C.

[0050] Figure 4 shows the average internal bond strength (IB) curve over time in seconds for cured resins from Comparative Examples A and B and Inventive Examples 1-3.

[0051] Figure 5 shows the average internal drying / pre-curing bond of Comparative Examples A and B and Inventive Examples 1-3.

[0052] Figure 6 shows the water tolerance and thickness swelling (WATS) of cured resins from Comparative Examples A and B and Inventive Examples 1-3.

[0053] Figure 7 shows formaldehyde emissions versus press cycle (90 - 370 seconds) for Comparative Examples A and B and Inventive Examples 1-3.

[0054] Figure 8 shows the process of producing lignosulfonates.

[0055] Figure 9 shows the differences between lignosulfonates and other lignin species.

[0056] Figure 10 shows a graph (not part of the previous artwork) comparing the internal bond strength. Petition 870260076067, dated 07 / 30 / 2026, page 23 / 62 18 / 53 measurement of a resin prepared from urea and formaldehyde (0% melamine) and a resin prepared from melamine, urea and formaldehyde (2% melamine).

[0057] Figure 11 shows the tensile strength in the dry state of a glass fiber nonwoven of the present invention compared with a glass fiber nonwoven lacking one or more lignosulfonate compounds.

[0058] Figure 12 demonstrates that the mixture of materials comprising one or more lignosulfonate salts can have a distinct color that is visibly different from the color of the resins. Pure UF / MUF. DETAILED DESCRIPTION OF THE INVENTION I. Definitions

[0059] The following terms are intended to have the meanings set forth below and are useful for understanding the description and intended scope of the present invention.

[0060] The articles a and an can be used here to refer to one or more of one (i.e., at least one) of the grammatical objects of the article. As an example, an analogue means an analogue or more than one analogue.

[0061] The term about, as used herein, refers to the fact that the numerical value is approximate and that small variations would not significantly affect the practice of the disclosed modalities. Where a numerical limitation is used, unless otherwise indicated in the context, about means that the numerical value may vary by ±10% and remain within the scope of the disclosed modalities. Additionally, in the expression, about X to Y is equal to about X to about Y, that is, the term about modifies both X and Y.

[0062] The term compound as used herein refers to salts, complexes, isomers, stereoisomers, diastereomers, tautomers and isotopes of the compound or any combination thereof. Petition 870260076067, dated 07 / 30 / 2026, page 24 / 62 19 / 53

[0063] The terms comprising (and any form of comprising, such as to comprise, comprises and comprised), having (and any form of having, such as to have and has), including (and any form of including, such as includes and to include), or containing (and any form of containing, such as contains and to contain), are used in their inclusive, open and non-limiting sense.

[0064] The term effective, as this term is used in the descriptive report and / or claims, means suitable for achieving a desired, expected or intended result.

[0065] The term coating refers to a coating in a form that is suitable for application to a substrate, as well as the material after it has been applied to a substrate, while it is being applied to the substrate, and both before and after any post-application treatments (such as evaporation, crosslinking, curing and the like). The components of coating compositions may vary during these stages. II. Mixture of materials

[0066] The invention provides methods and compositions for mixing materials.

[0067] In some embodiments, a mixture of materials may include a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin; a lignosulfonate or kraft lignin; an alkaline compound; optionally an additive; and a plurality of substrates, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

[0068] In certain embodiments, the substrate is selected from the group consisting of lignocellulose substrates, natural fiber substrates, synthetic fiber substrates, glass fiber substrates and mixtures thereof.

[0069] In other forms, lignosulfonate is Petition 870260076067, dated 07 / 30 / 2026, page 25 / 62 20 / 53 selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate and mixtures thereof.

[0070] In certain embodiments, lignosulfonate or kraft lignin is added to UF resin or MUF resin at a resin manufacturer's facility, at a lignosulfonate or kraft lignin supplier's facility, at a third-party supplier's location, in a wood-based composite manufacturer's storage tank, in a railcar, truck or other transport vehicle, or combinations thereof.

[0071] In additional embodiments, lignosulfonate or kraft lignin is mixed with other additives selected from the group consisting of crude lignin in powder or liquid form, lignin added to additives combined with additional water, urea water, a sequestrant, a filler, an extender, a wax, a catalyst, a release agent, a buffering agent, a surfactant and mixtures thereof.

[0072] In certain embodiments, lignosulfonate or kraft lignin is added into the process in a digester (MDF), a blow line (MDF), a mixer (PB), a high-jet application system (PB / MDF), a refiner (MDF), a belt sprayer (PB / MDF - end of the forming line), a moisture control (mixed with water), an extruder, or combinations thereof.

[0073] In another embodiment, lignosulfonate or kraft lignin is in solid powder form, liquid form, or combinations thereof.

[0074] In some embodiments, the alkaline compound may include ammonia, an amine, a Group I metal hydroxide, a Group II metal hydroxide, a Group I metal carbonate, a Group II metal carbonate, or combinations thereof. Petition 870260076067, dated 07 / 30 / 2026, page 26 / 62 21 / 53

[0075] In other embodiments, the additive is selected from the group consisting of catalyst, filler, buffer, base, tackifying agent, wax, water, sequestrant, boron compound, phosphate, halogen compound, nitrogen compound, and mixtures thereof.

[0076] In one embodiment, one or more additives are present.

[0077] In certain embodiments, the mixture of materials may include one or more lignosulfonate salts which may have a distinct color that is noticeably different from the color of the pure UF / MUF resins. Figure 12 demonstrates that the mixture of materials comprising one or more lignosulfonate salts may have a distinct color that is noticeably different from the color of the pure UF / MUF resins.

[0078] In other embodiments, the lignocellulose substrate may include a granular lignocellulose substrate, a flake lignocellulose substrate, a fibrous lignocellulose substrate, or combinations thereof.

[0079] In additional embodiments, the material mixture may include from about 0.0% by weight to about 50% by weight of UF resin or MUF resin; from about 0.1% by weight to about 30% by weight of lignosulfonate or kraft lignin; from about 0.0% by weight to about 1% by weight of alkaline compound; and from about 0.0% by weight to about 40% by weight of additive, wherein each percentage by weight is based on the total weight of the material mixture.

[0080] In certain embodiments, lignosulfonate or kraft lignin is mixed with a catalyst, a filler, a buffer, a base, a tackifying agent, wax, water, a sequestrant, a boron compound, a phosphate, a halogen compound, a nitrogen compound, and mixtures thereof at the facilities of a resin manufacturer, at the lignosulfonate and kraft lignin supplier's facility, at a third-party supplier's location, or in a storage tank of a Petition 870260076067, dated 07 / 30 / 2026, page 27 / 62 22 / 53 manufacturer of wood-based composites, in a railway wagon, in a truck or other transport vehicle or combinations thereof. III. Methods of manufacturing material mixtures

[0081] The invention provides methods for manufacturing and using a mixture of materials.

[0082] In some embodiments, a method for preparing a mixture of materials may include adding a plurality of substrates; mixing a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin optionally with an amine and water to a pH of 5-11, preferably 6-10; optionally adding one or more additives; adding a lignosulfonate salt or a kraft lignin; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

[0083] In certain embodiments, the lignosulfonate is selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate and mixtures thereof.

[0084] In other embodiments, a method for preparing a mixture of materials may include adding a plurality of substrates; mixing a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin, a lignosulfonate salt or a kraft lignin optionally with an amine and water to a pH of 5-11, preferably 6-10; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of Petition 870260076067, dated 07 / 30 / 2026, page 28 / 62 23 / 53 time of up to 20 days.

[0085] In additional embodiments, the lignosulfonate is selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate and mixtures thereof.

[0086] In some embodiments, a method for preparing a mixture of materials may include adding a plurality of substrates; mixing a lignosulfonate salt or kraft lignin with the substrates; adding a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin, optionally with an amine and water at a pH of 5-11, preferably 6-10; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

[0087] In other embodiments, the lignosulfonate is selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate and mixtures thereof. IV. Composite product

[0088] The invention provides a composite product using a mixture of materials.

[0089] In some embodiments, a composite product may include a plurality of substrates; and a mixture of materials that is at least partially cured, wherein the mixture of materials, prior to curing, may include a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin; a lignosulfonate or a kraft lignin; an alkaline compound; and, optionally, one or more additives; wherein the mixture of materials has a Petition 870260076067, dated 07 / 30 / 2026, page 29 / 62 24 / 53 Buffer capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of material mixture over a period of up to 20 days.

[0090] In other embodiments, the composite product may include plywood, oriented strand board, oriented strand construction timber, laminated veneer construction timber, laminated veneer wood, laminated veneer panels, particleboard, fiberboard, chipboard, flakeboard, high-density fiberboard, medium-density fiberboard, wafer-type board, hardwood, softwood plywood, veneer wood, parallel pattern construction timber, oriented strand construction timber, or combinations thereof. V. Resin system

[0091] The present disclosure is directed to ready-to-use resin systems, applications containing the resin system, and methods of preparing the resin system. The resin system of the present invention contains urea and formaldehyde and, optionally, melamine. The present inventors have found that a partial to total replacement of melamine in melamine-urea-formaldehyde (MUF) resin systems with a weight equivalent of a lignosulfonate can produce a more environmentally friendly resin while maintaining the same resin performance. This is especially significant because lignosulfonates are an eco-friendly component.

[0092] The resin system of the present invention may include a UF resin or a MUF resin, prepared by: a urea-formaldehyde (UF) resin or melamine-urea-formaldehyde (MUF) resin, prepared by: Mix a first set of components comprising one or more urea compounds and one or more formaldehyde compounds and, optionally, one or more melamine compounds, optionally heating while mixing during Petition 870260076067, dated 07 / 30 / 2026, page 30 / 62 25 / 53 for at least one minute, to form a first reaction product having an initial molar ratio (IMR) of total moles of one or more formaldehyde compounds to moles of one or more urea compounds plus, if present, one or more melamine compounds of about 1.4:1 to 5:1, or about 1.4:1 to 3:1, or about 2; mix the first reaction product with a second set of components comprising one or more urea compounds and a buffering and stabilizing agent and, optionally, one or more melamine compounds; optionally heat while mixing to form a UF resin or a MUF resin, wherein the UF resin or the MUF resin has a molar ratio (IMR) of total moles of formaldehyde to total moles of urea plus, if present, one or more melamine compounds of about 0.25:1 to about 2.50:1, or about 0.25:1 to about 1.5:1, and if the pH of the UF resin or MUF resin is not from 6.5 to about 10.0, or from about 8.0 to about 10.0, or from about 8,0 to about 9.0, then one or more alkaline compounds may be mixed with the UF resin or the MUF resin until the pH of the UF resin or the MUF resin is from 6.5 to about 10.0, or from about 8.0 to about 10.0, or from about 8.0 to about 9.0 to form the resin system, in which one or more lignosulfonate compounds are included with the first set of components and / or with the second set of components in an amount of about, 0.1% by weight to about 30% by weight, or from about 1.0% by weight to about 20% by weight, or from about 1.0% by weight to about 10% by weight, based on a total weight of the resin system, about 0.0% by weight to about 40% by weight of water, based on the total weight of the resin system, and wherein the resin system has a buffer capacity of 2 to 400 mL, or greater than 5 to 150 mL, preferably 20 to mL of 0.1 N HCl by the ATV method for a period of time of at least about 20 days at 25°C. Petition 870260076067, dated 07 / 30 / 2026, p. 31 / 62 26 / 53

[0093] UF or MUF resin is normally prepared in two stages. In the first stage, a first set of components, comprising one or more urea compounds and one or more formaldehyde compounds and, optionally, one or more melamine compounds, are heated while mixing for at least one minute, to form a first reaction product. Preferably, the first set of components is heated to a temperature of about 75°C to about 100°C, or about 80°C to about 95°C or about 85°C to about 90°C.

[0094] The first step in preparing UF or MUF resin is normally done using a molar excess of formaldehyde. One or more urea compounds, one or more formaldehyde compounds, and, if present, one or more melamine compounds are present in an amount such that the first reaction product has a molar ratio (MR) of total moles of one or more formaldehyde compounds to moles of one or more urea compounds plus, if present, one or more melamine compounds of about 1.4:1 to 5:1, or about 1.4:1 to 3:1, or about 2. The one or more urea compounds in the first set of components may be present in an amount of about 5% by weight to about 35% by weight, or about 10% by weight to about 30% by weight, or about 15% by weight to about 25% by weight, based on the total weight of the resin system.In some embodiments, one or more melamine compounds in the first set of compounds may include from about 0.1% by weight to about 20% by weight, or from about 1.0% by weight to about 15% by weight, or from about 2.0% by weight to about 5.0% by weight, or more than 2.0% by weight to about 5.0% by weight, wherein each percentage by weight is based on the total weight of the resin system. The total formaldehyde present in the resin system is from about 5% by weight to about 40% by weight, or from about 10% by weight to about 35% by weight, or from about 15% by weight to about 30% by weight, based on the total weight of the resin system. Petition 870260076067, dated 07 / 30 / 2026, page 32 / 62 27 / 53

[0095] In the second stage, the first reaction product is mixed with a second set of components comprising a urea compound, a buffering agent and a stabilizer. These components are all mixed and can be heated to a temperature of about 20°C to about 60°C, or about 25°C to about 55°C, or about 30°C to about 50°C, to form the UF or MUF resin.

[0096] Pure UF / MUF resins are normally clear or white. Sometimes there will be a yellowish tint which is due to iron contamination and oxidation of the additives that go into the resin. When lignosulfonate is added to the resin, the color change is obvious. There are different grades of lignosulfonate and its color changes depending on the region, wood species and lignin content. In each of the preceding embodiments, the resin system comprising one or more lignosulfonates has a color that is visibly different from the color of pure UF / MUF resins. Preferably, within 72 hours after the formation of the resin system, 1 liter of the resin system may exhibit an orange, yellow, red, beige or brown color; or in which, within 72 hours of resin system formation, the resin system may have a color that is in the range of 4 to 40+ using the official AIH SRM (Standard Research Method) numerical scale for beer color.

[0097] One or more urea compounds and, optionally, one or more melamine compounds of the second set of components are present in an amount such that the UF or MUF resin has a molar ratio (MR) of total moles of one or more formaldehyde compounds to total moles of one or more urea compounds and, if present, one or more melamine compounds of about 0.25:1 to about 2.50:1, or from about 0.25:1 to about 1.5:1. In some embodiments, one or more urea compounds in the second set of compounds may be present in an amount of about 15% by weight to about Petition 870260076067, dated 07 / 30 / 2026, p. 33 / 62 28 / 53 40% by weight, or from about 20% by weight to about 37% by weight, or from about 25% by weight to about 35% by weight, based on the total weight of the resin system. In some embodiments, one or more melamine compounds in the second set of compounds may include from about 0.1% by weight to about 20% by weight, or from about 1.0% by weight to about 15% by weight, or from about 2.0% by weight to about 5.0% by weight, or more than 2.0% by weight to about 5.0% by weight, where each percentage by weight is based on the total weight of the resin system.

[0098] The purpose of the final addition of urea is to sequester excess free formaldehyde. This is advantageous as it ensures that the resin system meets standard requirements for formaldehyde emissions. In some embodiments, during the second step, one or more urea compounds and, if present, one or more melamine compounds from the second set of components, are allowed to dissolve for about 5 minutes to about 1 hour, or about 30 minutes. Once one or more urea compounds and, if present, one or more melamine compounds are dissolved, the buffering and stabilizing agent can be added to the UF or MUF resin. The buffering and stabilizing agents may each be present independently in amounts ranging from about 0.0% by weight to about 20% by weight, or from about 0.001% by weight to about 3% by weight, or from about 0.01% by weight to about 2.0% by weight, based on the total weight of the resin system.

[0099] After that, an alkaline compound or an acidic compound can be added to the UF or MUF resin and mixed to adjust the pH of the resin. Preferably, the alkaline compound or acidic compound is added until a pH of about 6.5 to about 10.0, or about 8.0 to about 10.0, or about 8.0 to about 9.0 is achieved.

[00100] The alkaline compound can be a strong base. The incorporation of the alkaline compound aids in the overall stability of the resin, as the same resin system, without the compound Petition 870260076067, dated 07 / 30 / 2026, pp. 34 / 62 29 / 53 alkaline, results in gelation. As more alkaline compound is added, the pH increases and thus produces a more stable resin system.

[00101] The % of non-volatiles in the resin system may be in the range of about 40 to about 80, or about 50 to about 75, as measured via NATM-A12.

[00102] One or more urea compounds that may be used in the first or second set of components include, but are not limited to, dimethylol urea, methylated dimethylol urea, urea-resorcinol, and mixtures thereof.

[00103] One or more formaldehyde compounds that may be used in the first set of components include, but are not limited to, formaldehyde, paraformaldehyde, trioxane, acetaldehyde, glyoxal, glutaraldehyde, polyoxymethylene, propionaldehyde, isobutyraldehyde, benzaldehyde, acrolein, crotonaldehyde, furfural, 5-hydroxymethylfural, and combinations thereof. Formaldehyde is the most commonly used. Like the aldehyde, formalin in the form of an aqueous solution is optimal, but forms such as paraformaldehyde, benzaldehyde, trioxane, and tetraoxane may be used. It may be used by substitution with aldehyde or furfuryl alcohol.

[00104] The one or more melamine compounds that are optionally used in the first and / or second set of components include, but are not limited to, melamine, methylol melamine, methylated methylol melamine, imino melamine, and mixtures thereof. In some embodiments, the one or more melamine compounds may be added in up to a 1:1 molar ratio with the total moles of the one or more urea compounds in the resin system, or the one or more melamine compounds may be added in a molar ratio of 0.001:1 to 0.5:1 with the total moles of the one or more urea compounds in the resin system, or the one or more melamine compounds may be added in a molar ratio of 0.01:1 to 0.25:1 with the total moles of the one or more Petition 870260076067, dated 07 / 30 / 2026, page 35 / 62 30 / 53 urea compounds in the resin system.

[00105] Alkaline compounds may include, but are not limited to, one or more Group I or II metal hydroxides, one or more Group I or II metal carbonates, ammonia, one or more amines, or mixtures thereof. Suitable hydroxides may include, but are not limited to, sodium hydroxide, potassium hydroxide, ammonium hydroxide (e.g., aqueous ammonia), lithium hydroxide, cesium hydroxide, or any mixture thereof. Illustrative examples include lithium carbonate, ammonium carbonate, or any mixture thereof. Illustrative examples include trimethylamine, triethylamine, triethanolamine, diisopropylethylamine (Hunig base), pyridine, 4-dimethylaminopyridine (DMAP), 1,4-diazabicyclo[2.2.2]octane (DABCO), or any mixture thereof. Preferably, the alkaline compound can be selected from sodium hydroxide, potassium hydroxide, caustic soda, ammonium hydroxide, or any mixture thereof.Immediately after the formation of the UF or MUF resin, the alkaline compound is mixed with the UF or MUF resin to form the resin system.

[00106] As discussed above, an amount of alkaline compound can be added to the first set of components to ensure that the pH is in a range of 4-10, or an alkaline compound can be added to the second set of components to ensure that the pH is in a range of 6.5 to about 10.0, or about 8.0 to about 10.0, or about 8.0 to about 9.0 when forming the resin system to ensure stability and buffering capacity. Even so, after a certain duration of time following the formation of the resin system, an additional amount of alkaline compound can optionally be added to improve stability. The duration of time can be from about 1 to about 72 hours, or from about 2 hours to about 60 hours, or about 24 to 48 hours after Petition 870260076067, dated 07 / 30 / 2026, page 36 / 62 31 / 53 the formation of the resin system. The amount of alkaline compound can be added to the resin system until a pH of about 6.5 to about 10.0, or about 8.0 to about 10.0, or about 8.0 to about 9.0 is obtained.

[00107] Acidic compounds may include, but are not limited to, chloric acid, hydrobromic acid, hydrochloric acid, hydroiodic acid, nitric acid, perchloric acid, sulfuric acid, sulfurous acid, phosphoric acid, acetic acid, formic acid, benzoic acid, oxalic acid, hydrogen sulfate ion, nitrous acid, hydrofluoric acid, carbonic acid, methanoic acid, or any mixtures thereof.

[00108] As discussed above, a quantity of acidic compounds can be added to the second set of components to ensure that the pH is in a range of 6.5 to about 10.0, or about 8.0 to about 10.0, or about 8.0 to about 9.0, when forming the resin system to ensure stability and buffering capacity.

[00109] The UF resin further comprises a lignosulfonate which may be included either in the first set of components or with the second set of components, in an amount of about 0.1% by weight to about 30% by weight, or about 1.0% by weight to about 15% by weight, or about 2.0% by weight to about 5.0% by weight, or more than 2.0% by weight to about 5.0% by weight, based on the total weight of the resin system.

[00110] In embodiments where lignosulfonate is included in the first set of components, the lignosulfonate, one or more urea compounds, total formaldehyde and, if present, one or more melamine compounds from the first set of components, are mixed and heated together. In embodiments where lignosulfonate is included in the second set of components, the lignosulfonate is added after one or more urea compounds and, if present, one or more compounds of Petition 870260076067, dated 07 / 30 / 2026, page 37 / 62 32 / 53 melamine from the second set of components must be dissolved and the buffering and stabilizing agent added, but before the addition of the alkaline compound.

[00111] Lignosulfonate can be extracted, separated, or otherwise recovered from wood, plant, and / or vegetable matter using any of several well-established processes. For example, in the pulp and paper industry, lignin-containing materials such as wood, straw, corn stalks, bagasse, and other plant and vegetable tissues can be processed to recover cellulose pulp through the well-known sulfite process. Residual pulping liquors that include lignin as a byproduct can be a source of lignin. The chemical structure of lignin can vary, and the variation may depend, at least in part, on the particular plant from which the lignin is recovered, the location where the plant was grown, and / or the particular method used in recovering or isolating the lignin from the plant and / or vegetable matter.Lignin may include active groups, such as active hydrogens and / or phenolic hydroxyl groups, through which crosslinking or bridging can be effected.

[00112] A process for recovering lignin may include the process commonly known as the organosolv process. The organosolv process uses an organic solvent to solubilize lignin and hemicelluloses. The organosolv process may involve contacting lignocellulose material, for example, wood chips or particles, with an aqueous organic solvent at a temperature of about 130°C, about 140°C, or about 150°C to about 200°C, about 220°C, or about 230°C. The lignin may break down by hydrolytic cleavage of alpha aryl-ether linkages into fragments that can be solubilized in the solvent system. Illustrative solvents may include, but are not limited to, acetone, methanol, ethanol, butanol, ethylene glycol, formic acid, acetic acid, or any mixture thereof. The Petition 870260076067, dated 07 / 30 / 2026, pp. 38 / 62 33 / 53 aqueous organic solvent may have a solvent concentration in water of about 30% by weight, about 40% by weight or about 50% by weight to about 70% by weight, about 80% by weight, or about 90% by weight.

[00113] Because lignin separated from the plant can be chemically altered from that found in the plant, the term lignin can also refer to lignin products obtained after separation from cellulose or recovered from plant matter. For example, in a sulfite pulping process, lignocellulosic material can be digested with a bisulfite or sulfite, resulting in at least partial sulfonation of the lignin. As such, lignin can optionally be subjected to further cleavage and / or other modifications, such as alkaline treatment or reaction with other constituents to decrease the sulfonate or sulfur content and / or increase the active groups.

[00114] The liquors from which lignin can be recovered may also include one or more other constituents besides lignin. For example, in the sulfite pulping process, spent sulfite liquor may include lignosulfonates which may be present as salts of cations such as magnesium, calcium, ammonium, sodium, potassium and / or other cations. The solids of spent sulfite liquor may include about 40% by weight to about 65% by weight of lignosulfonates, the remainder being carbohydrates and other organic and inorganic constituents dissolved in the liquor.

[00115] Preferably, the lignin employed in the present invention is prepared from the sulfite pulping process to produce a lignosulfonate. This process is illustrated in Figure 8. Preferably, the resin system does not include lignin species, such as kraft lignin. Figure 9 demonstrates the differences in the pulping process for preparing lignosulfonates compared with lignin species.

[00116] Suitable examples of lignosulfonates may be Petition 870260076067, dated 07 / 30 / 2026, pp. 39 / 62 34 / 53 selected from calcium lignosulfonate, magnesium lignosulfonate, ammonium lignosulfonate, or sodium lignosulfonate, or preferably ammonium lignosulfonate or sodium lignosulfonate. The lignosulfonates in the resin system may have a weight-average molecular weight of about 1,000 daltons to about 100,000 daltons, as measured by gel permeation chromatography (GPC). For example, lignosulfonate may have a weight-average molecular weight of about 5,000 daltons to about 80,000 daltons, or about 15,000 to about 80,000 daltons, or about 30,000 to about 70,000 daltons, or about 50,000 to about 70,000 daltons, as measured by gel permeation chromatography (GPC). Resin system lignosulfonates may have a number-average molecular weight of about 50 daltons to about 25,000 daltons, or about 5,000 daltons to about 25,000 daltons, or about 12,000 daltons to about 20,000 daltons.000 daltons, as measured by gel permeation chromatography (GPC). The lignosulfonates in the resin system may have a polydispersity (Mw / Mn) of about 1 to about 100, or greater than 1 to about 20, or from about 2 to 8. Preferably, lignin species, such as kraft lignin, are not added to the resin system.

[00117] The lignosulfonates of the present invention may include from about 1% by weight to about 20% by weight of sulfur, or from about 1.5% by weight to about 15% by weight of sulfur, or from about 3% by weight to about 10% by weight of sulfur, based on the weight of the lignosulfonate.

[00118] Buffer and stabilizing agents can be used to stabilize the pH of a solution, that is, they resist changes in pH when acidic or alkaline materials are added to the solution. Suitable buffer and stabilizing agents can be selected from glycine hydrochloride, sodium acetate, phosphate-buffered saline (PBS). Petition 870260076067, dated 07 / 30 / 2026, pages 40 / 62 35 / 53 (including mono- and dihydrogen phosphate sheets), citrate buffer (citric acid and sodium citrate), phosphate-citrate buffer, tris(hydroxymethyl)aminomethane (tris), carbonate buffers, borate buffers, borate-buffered saline solution, magnesium chloride, potassium chloride, zinc chloride, hydrochloric acid, sodium hydroxide, disodium edetate, various substituted amines (alkylamines, aliphatic and aromatic diamines and triamines) and their salts, sodium formate, sodium sulfate, phosphate salts (potassium mono-, di- and tri-basic), and combinations thereof.

[00119] Buffering and stabilizing agents may be present in amounts of 0.001% by weight to 20% by weight, or 0.001% by weight to 2% by weight, or 0.01% by weight to 1.0% by weight, based on the total weight of the resin system.

[00120] The UF or MUF resin, excluding lignosulfonate, may have a number-average molecular weight (Mn) of about 300 daltons to about 20,000 daltons, or about 1,000 daltons to 10,000 daltons, or about 1,500 daltons to about 9,000 daltons, as measured by gel permeation chromatography (CPG). The UF or MUF resin, excluding lignosulfonate, may have a weight-average molecular weight of about 30,000 to about 200,000 daltons, as measured by gel permeation chromatography (CPG). The UF or MUF resin, excluding lignosulfonate, may have a polydispersity (Mw / Mn) of about 10 to about 100.

[00121] The resin system of the present invention has a suitable buffering capacity of 2-400 mL, or greater than 5 to 150 mL, preferably 20-60 mL of 0.1 N HCl by the ATV method for a period of at least about 20 days at 25°C. Well-known MUF resin systems cannot be simply modified to replace some or all of the melamine with lignosulfonate to achieve compositions of the same quality; thus, other components, such as a Petition 870260076067, dated 07 / 30 / 2026, pp. 41 / 62 36 / 53 buffering and stabilizing agent and alkaline compound are preferred. These components ensure that the resin system obtains the appropriate buffering capacity. A very low buffering capacity results in an unstable material that will cure too early and dry out, but a very high buffering capacity cures too slowly in the press, losing the material's effectiveness.

[00122] The viscosity of the resin system can vary widely depending on the amount of time elapsed since the time of manufacture. For example, the kinematic viscosity of the resin system can be in the range of about 100 to about 1,500 cSt, or about 100 to about 1.000 cSt, or about 100 to about 600 cSt at a temperature of about 250°C, as measured by the Gardner-Holdt viscosity method, over a period of at least about 20 days at 250°C, wherein the period of time begins when the resin system is initially produced, and the resin system may have a rapid cure rate so as to achieve an improvement in internal bond strength when compared to the control resin system of up to 20%, preferably 10% to 20% at < 7.0 press factor at a plate temperature of 350°F (176.6°C), when measured at full cure at < 7.0 press factor at a plate temperature of 350°F (176.6°C), the internal bond strength (IB) is at least as good for the inventive resin as compared to the comparator resin. The control resin is Comparative Example B, discussed below.

[00123] The Gardner-Holdt (bubble) viscosity method allows for a rapid determination of the kinematic viscosity of liquids, such as resins and varnishes. Certified Gardner tubes can be used for viscosity measurement at room temperature, approximately 25°C. The Gardner-Holdt (bubble) viscosity method may include a scale that is in the range A4 - Z6, corresponding to a kinematic viscosity range of 10 cSt to approximately 15,000 cSt at 25°C, as measured by a Brookfield viscometer with a Petition 870260076067, dated 07 / 30 / 2026, pp. 42 / 62 37 / 53 small sample adapter, such as a 10 mL adapter, and the appropriate spindle to maximize torque, such as a No. 31 spindle. Appropriate values ​​for the viscosity of the resin system may include D-U or, preferably, H-S, via the Gardner-Holdt scale. Table 2 shows the Gardner-Holdt viscosity scale (bubble) with its corresponding kinematic viscosities, as measured by the Brookfield viscometer with a 10 mL adapter and No. 31 spindle: TABLE 1 cSt at 250C Gardner-Holdt Scale 100 D 120 E 140 F 160 G 200 H 220 I 240 J 280 K 300 L 320 M 340 N 360 O 400 P 440 Q 460 R 500 S 550 T 600 U

[00124] The resin system may also optionally include a quantity of melamine. Melamine may be present in an amount of about 0.0% by weight to about 30% by weight, or about 0.0% by weight to about 25% by weight, or about 0.0% by weight to about 20% by weight, or about 0.1% by weight to about 15% by weight, based on the total weight of the resin system. In some embodiments, no melamine. Petition 870260076067, dated 07 / 30 / 2026, pp. 43 / 62 38 / 53 is added to the resin composition.

[00125] In some embodiments, the UF or MUF resin may optionally be prepared with water. Water may be present in the resin system in an amount to provide from about 0.0% by weight to about 40% by weight, or from about 0.0% by weight to about 9% by weight, or from about 0.01% by weight to about 2% by weight, based on the total weight of the resin system. In embodiments where water is present, the water is included with either the first set of components or with the second set of components. The resin systems, as disclosed herein, employ low levels of water compared to the well-known urea-formaldehyde resins in the art. Typically, water is included to reduce the viscosity of a resin system and to aid in heat transfer from the product surface during the curing step.However, the combination of components in certain ratios of the present disclosure allows the resin systems to achieve an appropriate viscosity without the addition of large quantities of water.

[00126] The resin system may optionally include additional additives, such as primary, secondary and tertiary amines, for example, triethanolamine, organic and inorganic salts, and metal hydroxides.

[00127] The resin system discussed above can be used as adhesives, which can then be used to manufacture composite products. For example, the present invention also relates to a mixture of materials including a plurality of granular or fibrous lignocellulose substrates and an adhesive comprising resin systems.

[00128] The adhesives of the present invention may include additional components, such as fillers, extenders, organic and inorganic salts, organic polyols and additives based on carbohydrates, acrylics and organic proteins.

[00129] Suitable fillers may include, but are not. Petition 870260076067, dated 07 / 30 / 2026, pp. 44 / 62 39 / 53 limited to, walnut shell medium, corn medium or corn cob medium, furfural residue, or any mixture thereof. Walnut shell medium may be or include whole, broken, chopped, crushed, ground shells, and / or clusters of nuts and / or seeds. Suitable shelled nut mediums may include, but are not limited to, almond, walnut, pecan, chestnut, pecan, cashew, peanut, macadamia, or any mixture thereof. Corn medium may be or include broken, chopped, crushed or ground corn cobs, corn stalks or other corn-derived products, or any mixture thereof. Corn medium may also include furfural residue from corn cobs, corn stalks or other corn-derived products.An illustrative corn-derived product may include, but is not limited to, a cellulose byproduct derived from the manufacture of furfural, or furfural residues, including compounds derived from florets and furfural; it may also be derived from oats, wheat, wheat bran, barley, wood particles, sawdust, and / or other plant-based products. Illustrative seed husks (including fruit pits) may include, but are not limited to, the seed husks or pits of fruits, for example, plum, peach, cherry, apricot, olive, mango, jackfruit, guava, custard apple, pomegranate, pumpkin, melon; ground or crushed seed husks of other plants such as corn, wheat, rice, sunflower, or similar, or any mixture thereof. Other examples of suitable fillers include, but are not limited to, wheat husks, corn cob husks, peanut husks, or any combination thereof.

[00130] Suitable extenders may include, but are not limited to, one or more flours, one or more polysaccharides, one or more starches, one or more polysaccharide starches, or any mixture thereof. Flours may be milled or ground into a variety of different granular sizes, Petition 870260076067, dated 07 / 30 / 2026, pages 45 / 62 40 / 53 as fine, ultrafine, or very ultrafine. Illustrative flours may include, but are not limited to, wheat flour, corn flour, soy flour, oat flour, other grain flours, nut or seed flour (e.g., almond, walnut, pecan, cashew, or peanut), types thereof, starches thereof, or any mixture thereof. In some examples, the extender may be or include corn flour or corn starches, such as NCS-83, NCS-74, and 4501 flour, commercially available from Didion Milling Company, Inc., Sun Prairie, WI. In other examples, the extender may be or include wheat flours, wheat starches, and / or wheat-derived protein-starch composition. Illustrative polysaccharides may include, but are not limited to, starch, cellulose, gums such as guar and xanthan gum, alginates, pectin, gellan, or any mixture thereof.Suitable polysaccharide starches may include, for example, maize or corn, native corn starch (NCS), waxy maize, high-amylose maize, potato, tapioca, wheat starch, or any mixture thereof. Other starches, such as genetically modified starches, may include high-amylose potato starches, potato amylopectin starches, or any mixture thereof.

[00131] In one or more embodiments, the method for manufacturing a lignocellulosic composite product may include contacting a plurality of lignocellulose substrates and a partially cured resin system, as disclosed above. The resin system may be at least partially cured, for example, by heating, to produce the composite product. The lignocellulosic composite product may also include, but is not limited to, extender, filler, or any mixture thereof.

[00132] Heating the resin system can cause or promote at least partial curing of the resin system to produce the composite product. As used herein, the terms curing, Petition 870260076067, dated 07 / 30 / 2026, pages 46 / 62 41 / 53 cured, “at least partially curing”, “at least partially cured” and similar terms refer to the structural and / or morphological change that occurs in the mixture, such as by covalent chemical reaction (crosslinking), ionic interaction or clustering, transformation or phase inversion and / or hydrogen bonding, when subjected to sufficient conditions, i.e., sufficiently heated, to cause changes in the properties of a flexible and porous substrate, such as a non-woven blanket or covering of lignocellulose substrates, and / or a rigid or semi-rigid substrate, such as wood or other board or sheet containing lignocellulose, to which an effective amount of the adhesive has been applied.

[00133] In one or more embodiments, one or more additives may be combined with the adhesive and / or any one or more components of the adhesive to produce the composite product.

[00134] Illustrative additives may include, but are not limited to, waxes and / or other hydrophobic additives, release agents, colorants, flame retardants, formaldehyde scavengers, biocides, or any mixture thereof. In some examples, the mixtures, compositions, and products, including, but not limited to, the adhesive and the composite product, may be produced by a process of homogenization, agitation, mixing, combination, or other combination process, such as with homogenization, ultrasonication, colloidal milling, microfluidic mixing, as a homogenization method, or other similar processes.

[00135] Illustrative composite products may include, but are not limited to, plywood (e.g., hardwood plywood and / or softwood plywood), oriented strand board (OSB), laminated veneer wood (LVL), laminated veneer panels (LVB), engineered wood flooring, particleboard (PB), fiberboard (e.g., medium-density fiberboard (MDF) and / or fiberboard Petition 870260076067, dated 07 / 30 / 2026, pp. 47 / 62 42 / 53 high-density fiberboard (HDF), or other wood and non-wood products, preferably the composite product is a particleboard or medium-density fiberboard.

[00136] Illustrative products are not necessarily primarily wood-based and may include composites comprising the inventive resin system and glass mat and / or abrasives. The inventive resin system may be used in nonwoven fiberglass systems or as an impregnation resin in one or more layers of an overlay.

[00137] In some examples, the method may also include applying adhesive between two or more wood veneers or sheets of wood to produce the composite product (e.g., plywood, OSB, LVL, LVB, or engineered wood flooring). The plurality of lignocellulose substrates may be or include wood veneers or wood sheets, and the adhesive may be disposed between the wood veneers or wood sheets. In other examples, the method may also include forming a mixture of lignocellulose adhesives or resinous materials by combining the plurality of lignocellulose substrates and the adhesive and heating the adhesive to produce the composite product (e.g., particleboard, MDF, or HDF). EXAMPLES

[00138] The following examples are illustrative, but not limiting, of the methods and compositions of the present disclosure. Other modifications and adaptations appropriate to the variety of conditions and parameters normally encountered in the field, and which are obvious to those skilled in the art, are within the spirit and scope of the disclosure. All patents and publications cited herein are incorporated by reference in their entirety.

[00139] To demonstrate whether replacing melamine with an environmentally friendly lignosulfonate in melamine-urea formaldehyde resin provides comparable properties, five different resin systems are tested for resistance to Petition 870260076067, dated 07 / 30 / 2026, pp. 48 / 62 43 / 53 internal linkage, pH stability, and buffering capacity. Inventive Example 1 - UF resin with lignosulfonate (subsequent addition)

[00140] In a container, a first set of components is mixed. 40-50 parts of formaldehyde (52.5% solution) are combined with 0.01-0.1 parts of triethanolamine, and 0.5-1.5 parts of water. The temperature is maintained in the range of 50°C to 80°C and the pH is maintained between 8-10 with acid or base, as needed. 20-30 parts of urea are added and the temperature is increased in the range of 80°C to 110°C and the pH is maintained between 4-8 with acid or base, as needed. The second set of components is then added. The temperature is lowered to be in the range of 40°C to 80°C and 25-50 parts of urea, 1.0-5.0 parts of a first lignosulfonate salt and 0.01-0.1 parts of one or more buffering and stabilizing agents are mixed. The final pH is maintained between 8-10 with acid or base, as needed. Inventive Example 2 - UF resin with lignosulfonate (subsequent addition)

[00141] The process described above for Inventive Example 1 is essentially repeated, except that a different lignosulfonate salt is used. Inventive Example 3 - UF resin with lignosulfonate (previous)

[00142] In a container, a first set of components is mixed. 40-50 parts of formaldehyde (52.5% solution) are combined with 0.01-0.1 part of triethanolamine, 0.5-1.5 part of water and 1-5 parts of the same lignosulfonate salt used in Inventive Example 2. The temperature is maintained in the range 50°C to 80°C and the pH is maintained between 8-10 with acid or base as needed. 20-30 parts of urea are added and the temperature is increased in the range of 80°C to 110°C and the pH is maintained between 4-8 with acid or base as needed. The second set of components is then added. The temperature is decreased to be in the range of 40°C to 80°C and 25-50 parts of urea and 0.01-0.1 Petition 870260076067, dated 07 / 30 / 2026, pp. 49 / 62 44 / 53 of one or more buffering and stabilizing agents are mixed. The final pH is maintained between 8-10 with acid or base, as needed. Inventive Example 4 - MUF Resin with Lignosulfonate (previous)

[00143] In a container, a first set of components is mixed. 40-50 parts of formaldehyde (52.5% solution) are combined with 0.01-0.1 parts of triethanolamine, 0.5-1.5 parts of water, 1-5 parts of melamine, and 1-5 parts of lignosulfonate salt. The temperature is maintained in the range of 50°C to 80°C and the pH is maintained between 8-10 with acid or base as needed. 20-30 parts of urea are added and the temperature is increased in the range of 80°C to 110°C and the pH is maintained between 4-8 with acid or base as needed. The second set of components is then added. The temperature is lowered to be in the range of 40°C to 80°C and 25-50 parts of urea and 0.01-0.1 parts of one or more buffering and stabilizing agents are mixed. The final pH is maintained between 8-10 with acid or base, as needed. Comparative Example A - Lignosulfonate-free MUF resin

[00144] The process described above for Inventive Example 3 is essentially repeated, except that the 1-5 parts of lignosulfonate are replaced by 1-5 parts of melamine. In this Comparative Example A, lignosulfonate is not used. Comparative Example B - UF resin without melamine or lignosulfonate

[00145] The process described above for Inventive Example 2 is essentially repeated, except that no lignosulfonate is used. In this Comparative Example B, neither lignosulfonate nor melamine is used.

[00146] Samples were tested and the following results were obtained. TABLE 2 Example Example Example Example Example Comparative Comparative Inventive Inventive Inventive AB 1 2 3 Petition 870260076067, dated 07 / 30 / 2026, pages 50 / 62 45 / 53 Refractive index 1.4697 1.4671 1.4699 1.4701 1.4685 % Non-volatile 64.3 63.8 64.7 65.0 64.2 Final pH 8.53 8.59 8.69 8.91 8.34 Kinematic viscosity (cSt) 198 211 294 274 233 Buffer capacity (mL 0.1 N HCl) 19.2 10.5 18.8 15.0 14.1 Appearance Clear Clear Dark reddish-brown Dark reddish-brown Dark reddish-brown Color (AIH SRM) N / AN / A 32 31 31

[00147] The refractive index is measured by a digital refractometer.

[00148] The % of non-volatiles is measured via NATM-A12. A sample of liquid resin is cured in an aluminum pan in a convection oven with airflow at 105°C for 3 hours.

[00149] The viscosity of each resin is determined immediately after the final pH is reached using the Brookfield viscosity method (NATM-B01 / ASTM-D1084), at 25°C. See Table 2. Figures 1 and 2 show the viscosity stability over time for Comparative Examples A and B and Inventive Examples 1-3 at 25°C and 35°C, respectively. As seen from these graphs, Inventive Examples 1, 2, and 3 comprising melamine-free lignosulfonate provide similar viscosity stability when compared with Comparative Examples A and B. The viscosity of the resin system is stable so as to vary no more than 100 cSt at 25°C for at least 20 days, preferably at least 25 days, more preferably about 20 to 48 days. Figure 3 shows the pH decay over time for Inventive Examples 1-3 and Comparative Examples A and B at 25°C. As seen from these results, Inventive Examples 1-3 and Comparative Examples A and Petition 870260076067, dated 07 / 30 / 2026, pp. 51 / 62 46 / 53 B demonstrated similar pH stability. Given that the inventive resin system exhibits viscosity stability, it can be transported in a single container as a mixture to the customer without concern for component separation.

[00150] To determine the buffering capacity, each of the resins was measured by the acid titration value (ATV). The ATV method is performed by collecting 40.0 ± 0.1 grams of resin material in a beaker. 150 mL of a 50:50 volume mixture of isopropyl alcohol:water was added to the beaker with resin and mixed. The solution was then titrated with increments of 0.1 mL of HCl. The buffering capacity was determined by the mL of 0.1 mL of HCl required to obtain a pH of 4.0. The results are shown in Table 2.

[00151] Buffer capacity will depend on the system and can be manipulated so as not to be too high or too low, to ensure an appropriate balance between cure speed and resistance to pre-cure drying. Buffer capacity can be adapted to be optimized for a particular apparatus used to incorporate the inventive resin system into the product. Buffer capacity requirements are dependent on the resin stoichiometry and the customer's process. Both lignosulfonate and melamine content contribute to greater buffer capacity. The buffer capacity of the resin system is stable and will not be outside the range of 2-400 mL, or greater than 5 to 150 mL, preferably 20-60 mL of 0.1 N HCl by the ATV method at 25°C for at least 20 days, preferably at least 25 days, more preferably about 20-48 days.

[00152] To determine the color, within 72 hours of resin system formation, the colors of the resins were measured using the official AIH SRM (Standard Research Method) numerical scale for beer color.

[00153] Homogeneous particle panels were prepared Petition 870260076067, dated 07 / 30 / 2026, pages 52 / 62 47 / 53 by mixing each of Inventive Examples 1 to 3 and Comparative Examples A and B with a Douglas fir veneer. The resins were applied via a compressed air spray gun for atomization. Each panel was pressed in a laboratory hot pneumatic press with a single opening, at increasing pressing cycle times to obtain a cure curve and determine the relative cure rate and development of internal bond strength.

[00154] Table 3 shows the parameters for the preparation of particleboard panels. TABLE 3 Thickness: 0.570 inch (1.4478 cm) points. Plate temperature: 350°F (176.6°C). Resin filler: 10% by weight. Sequestrant: 0%. Target moisture content of the mix: 9 - 10%. Effective: Average 9.4%. Density: Target 45 lbs / ft3 (720.83 kg / m3). Effective (at full cure): 43.5 - 44.7 lbs / ft3 (696.8 kg / m3 - 715.6 kg / m3). Cycle times: 90, 120, 150, 180, 210, 250 seconds. Drying temperatures: 140°F, 160°F, 180°F (60.0°C, 71.1°C, 82.2°C) following the drying protocol. All fully cured (250 s) Construction Homogeneous face material (3.7 - 3.9% moisture content) a - Resin filler percentage = % by weight of resin solids / % kiln-dried wood b - %BMC = %MC measured from resin + substrate after mixing. Target %BMC will change based on specific panel construction and customer process. c - Drying protocol = A resin-coated material is placed in a bag. Each resin is tested after keeping the resin-coated material in an oven at 140, 160, 180°F (60.0°C, 71.1°C, 82.2°C). All of the Petition 870260076067, dated 07 / 30 / 2026, pages 53 / 62 48 / 53 panels are pressed for 250 seconds. The resin-bonded material is placed in a bag to prevent excessively rapid moisture loss during oven placement. The bag is used because bagged resin-bonded material more accurately mimics the drying times observed in commercial equipment.

[00155] Particleboard panels are also tested for bond cure rate and drying / precure resistance. To determine the average internal bond, according to ASTM-D1037, the panels are pressed for 250 seconds. Figure 4 shows the average internal bond (IB) curve over time for cured Inventive Examples 1 to 3 and Comparative Examples A and B.

[00156] To evaluate the average internal bond strength (AIB) during the drying / pre-curing of the resins, the panels are placed in containers while increasing the temperature over a period of time from 1250°F (52.6°C) to approximately 160°F (71.1°C). Figure 5 shows the average internal bond strength results during the drying / pre-curing of Inventive Examples 1-3 and Comparative Examples A and B.

[00157] Average internal bonds (AIBs) in drying / precuring are lower than AIBs using the standard panel process (without heating the resin-coated material in the oven) due to loss of efficiency (bonding potential) from excess heat before pressing.

[00158] Figure 4 indicates that the resin composition including lignosulfonate can actually improve the internal bonding with respect to Comparative Example A, which comprises melamine. Thus, Inventive Examples 1-3 provide resins capable of achieving appropriate internal bonding ranges more quickly with lignosulfonates.

[00159] Typically, resins that cure very quickly would dry correspondingly at low temperatures. This is because the resin is exposed to high temperatures during a Petition 870260076067, dated 07 / 30 / 2026, pp. 54 / 62 49 / 53 time period before the apparatus is brought to curing temperatures. This premature curing causes the resin to lose strength after the curing stage, thus resulting in drying at lower temperatures. Based on this, it would be expected that Inventive Examples 1 to 3 would exhibit worse performance in the drying stage, since they experienced rapid curing. See Figure 4. However, Figure 5 indicates that Inventive Examples 1 to 3 exhibit similar drying rates when compared with Comparative Example A, comprising melamine.

[00160] To determine water-resistant properties, including water absorption and thickness swelling, the panels were submerged in water for a period of time according to ASTM-D1037. Density (weight and thickness) was measured before and after submersion to determine the change. Figure 6 shows the water tolerance and thickness swelling (WATS) of cured Comparative Examples A and B and Inventive Examples 1-3.

[00161] In addition to testing the panels for water resistance, the panels are tested for formaldehyde emissions. During the curing phase, the amount of formaldehyde volatilization is measured over time using ASTM-6007 and E1333.Figure 7 shows formaldehyde emissions versus press cycle (90 - 370 seconds) for Comparative Examples A and B and Examples. Inventive 1-3.

[00162] A glass fiber nonwoven was prepared by mixing glass fibers with the inventive resin system comprising 5% by weight of sodium lignosulfonate. A control sample (comparative example) was prepared by mixing the glass fibers with essentially the same resin system except without any lignosulfonate. The glass fiber was an Owens Corning product, OC 9501 having an average fiber length of 1.25 inches (3.175 cm). A white water dispersant (a polyacrylamide) was used. The resin system containing the glass fibers was cured at 230°C for 15 seconds to give Petition 870260076067, dated 07 / 30 / 2026, pages 55 / 62 50 / 53 an average base resin weight of 1.65 lbs / 100 sq ft (0.081 kg / m2). The average loss on ignition was 20.3%. The dry tensile strength of the glass fiber nonwoven products was tested on a ThwingAlbert tensile testing apparatus (150 kg load cell) and the results are shown in Figure 11. The dry tensile strength shows that the inventive glass fiber nonwoven had approximately a 25-30% improvement in dry tensile strength compared to the control (comparative) example.

[00163] It is possible, and sometimes preferred, to use components in a diluted form. These include, but are not limited to, urea, formaldehyde, and melamine. All weight percentages described herein, unless otherwise indicated, are based on the weight of the component relative to the total weight (liquids and solids) of the resin system. For example, if 2 grams of a 50% by weight aqueous urea solution are added to the resin system to give a total weight of 10 grams, then the urea would be present in the resin system in an amount of 10% by weight.

[00164] Other embodiments of the present disclosure will be apparent to those skilled in the art from consideration of the descriptive report and practice of the embodiments disclosed herein. As used throughout the descriptive report and claims, a and / or an may refer to one or more of an. Unless otherwise indicated, all numbers expressing quantities of ingredients, properties such as molecular weight, percentage, ratio, reaction conditions, and so forth, used in the descriptive report and claims, shall be understood as being modified, in all cases, by the term about, regardless of whether the term about is present or not. Consequently, unless otherwise indicated, the numerical parameters specified in the description and claims are approximations that may vary depending Petition 870260076067, dated 07 / 30 / 2026, pages 56 / 62 51 / 53 of the desired properties sought to be obtained by the present disclosure. At a minimum, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be interpreted in light of the reported number of significant digits and by applying common rounding techniques. Although the ranges and numerical parameters specifying the broad scope of the disclosure are approximations, the numerical values ​​specified in the specific examples are reported to the greatest extent possible. Any numerical value, however, inherently contains certain errors, necessarily resulting from the standard deviation found in its respective test measurements. The descriptive report and examples are intended to be considered only as exemplary, with the true scope and spirit of the disclosure being indicated by the following claims.

[00165] The preceding embodiments are susceptible to considerable variations in practice. Consequently, the embodiments are not intended to be limited to the particular examples as specified above. Rather, the preceding embodiments are within the spirit and scope of the appended claims, including the equivalents thereof available as a matter of law.

[00166] The patent holders do not intend to dedicate any of the disclosed embodiments to the public and, to the extent that any disclosed modifications or alterations do not fall literally within the scope of the claims, they are considered an integral part thereof, in accordance with the doctrine of equivalents.

[00167] It should be understood that each component, compound, substituent or parameter disclosed herein should be interpreted as being disclosed for use alone or in combination with one or more of each of the other components, compounds, substituents Petition 870260076067, dated 07 / 30 / 2026, pp. 57 / 62 52 / 53 or parameters revealed here.

[00168] It should also be understood that each quantity / value or range of quantities / values ​​for each component, compound, substituent, or parameter disclosed herein shall be interpreted as also being disclosed in combination with each quantity / value or range of quantities / values ​​disclosed for any other component(s), compound(s), substituent(s), or parameter(s) disclosed herein, and that any combination of quantities / values ​​or ranges of quantities / values ​​for two or more component(s), compound(s), substituent(s), or parameters disclosed herein are therefore also disclosed in combination with each other for the purposes of this description.

[00169] It is further understood that each range disclosed herein shall be interpreted as a disclosure of each specific value within the disclosed range that has the same number of significant digits. Thus, a range of 1-4 shall be interpreted as an express disclosure of the values ​​1, 2, 3, and 4.

[00170] It is further understood that each lower limit of each range disclosed herein shall be interpreted as disclosed in combination with each upper limit of each range and each specific value within each range disclosed herein for the same component, compound, substituent, or parameter. Thus, this disclosure shall be interpreted as a disclosure of all ranges derived from the combination of each lower limit of each range with each upper limit of each range or with each specific value within each range, or from the combination of each upper limit of each range with each specific value within each range.

[00171] Furthermore, specific quantities / values ​​of a component, compound, substitute, or parameter revealed in the description or in an example should be interpreted as a disclosure of a lower limit or an upper limit of a Petition 870260076067, dated 07 / 30 / 2026, pages 58 / 62 53 / 53 range and thus may be combined with any other lower or upper limit of a range or specific quantity / value for the same component, compound, substitute or parameter disclosed elsewhere in the application to form a range for that component, compound, substitute or parameter. Petition 870260076067, dated 07 / 30 / 2026, pp. 59 / 62

Claims

1 / 5 CLAIMS 1. A mixture of materials, characterized in that it comprises: a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin; a lignosulfonate or kraft lignin; an alkaline compound; optionally an additive; and a plurality of substrates, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials for a period of up to 20 days.

2. A mixture of materials according to claim 1, characterized in that the substrate is selected from the group consisting of lignocellulose substrates, natural fiber substrates, synthetic fiber substrates, glass fiber substrates, and mixtures thereof.

3. A mixture of materials according to claim 1, characterized in that the lignosulfonate is selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate, and mixtures thereof.

4. Mixture of materials, according to claim 1, characterized in that lignosulfonate or kraft lignin is mixed with other additives selected from the group consisting of crude lignin in powder or liquid form, lignin added to additives combined with additional water, urea water, a sequestrant, a filler, an extender, a wax, a catalyst, a release agent, a buffering agent, a surfactant and mixtures thereof.

5. Mixture of materials according to claim 1, characterized in that the lignosulfonate or kraft lignin is in solid powder form, liquid form or combinations thereof.

6. Mixture of materials according to claim 1, characterized in that the alkaline compound comprises ammonia, an amine, a Group I metal hydroxide, a Group II metal hydroxide, a Group I metal carbonate, a Group II metal carbonate, or combinations thereof.

7. A mixture of materials according to claim 1, characterized in that the additive is selected from the group consisting of catalyst, filler, buffer, base, adhesion additive, wax, water, sequestrant, boron compound, phosphate, halogen compound, nitrogen compound, and mixtures thereof.

8. A mixture of materials according to claim 1, characterized in that one or more additives are present.

9. Mixture of materials according to claim 1, characterized in that the pH of the mixture of materials varies from about 3.0 to about 10.

0.

10. Mixture of materials, according to claim 1, characterized in that the mixture of materials comprising one or more lignosulfonate salts may have a distinct color that is visibly different from the color of pure UF / MUF resins.

11. Mixture of materials, according to claim 1, characterized in that the lignocellulose substrate comprises a granulated lignocellulose substrate, a flake lignocellulose substrate, a fibrous lignocellulose substrate or combinations thereof.

12. Mixture of materials, according to claim 1, characterized in that the mixture of materials comprises about 0.0% by weight to about 50% by weight of UF resin or MUF resin; about 0.1% by weight to about 30% by weight of lignosulfonate or kraft lignin; about 0.0% by weight to about 1% by weight of alkaline compound; and about 0.0% by weight to about 40% by weight of additive, wherein each percentage by weight is based on the total weight of the mixture of materials.

13. Method for preparing a mixture of materials, characterized in that it comprises: adding a plurality of substrates; mixing a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin optionally with an amine and water to a pH of 5-11, preferably 6-10; optionally adding one or more additives; adding a lignosulfonate salt or kraft lignin; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials for a period of up to 20 days.

14. Method according to claim 13, characterized in that the lignosulfonate is selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate and mixtures thereof.

15. Method for preparing a mixture of materials, characterized in that it comprises: adding a plurality of substrates; mixing a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin, a lignosulfonate salt or a kraft lignin optionally with an amine and water to a pH of 5-11, preferably 6-10; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials for a period of up to 20 days.

16. Method according to claim 15, characterized in that the lignosulfonate is selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate and mixtures thereof.

17. Method for preparing a mixture of materials, characterized in that it comprises: adding a plurality of substrates; mixing a lignosulfonate salt or kraft lignin with the substrates; adding a urea-formaldehyde (UF) resin or a melamine-urea-formaldehyde (MUF) resin, optionally with an amine and water to a pH of 5-11, preferably 6-10; optionally adding one or more additives to form the mixture of materials, wherein the mixture of materials has a buffering capacity of 2-200 mL of 0.1 N HCl by the acid titration value (ATV) method using 20 grams of the mixture of materials over a period of up to 20 days.

18. Method according to claim 17, characterized in that the lignosulfonate is selected from the group consisting of calcium lignosulfonate, magnesium lignosulfonate, potassium lignosulfonate, chromium lignosulfonate, ammonium lignosulfonate, sodium lignosulfonate and mixtures thereof.

19. Composite product, characterized in that it comprises: a plurality of substrates; and a mixture of materials at least partially cured as defined in claim 1.

20. Composite product, according to claim 19, characterized in that the composite product comprises plywood, oriented strand board, oriented strand construction timber, laminated veneer construction timber, laminated veneer wood, laminated veneer panels, particleboard, fiberboard, chipboard, flakeboard, high-density fiberboard, medium-density fiberboard, wafer-type panel, hardwood, softwood plywood, veneer wood, parallel pattern construction timber, oriented strand construction timber, or combinations thereof. Petition 870250071805, dated 08 / 14 / 2025, p. 22 / 25

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