CARBON-BASED PRODUCTS AND METHODS OF MANUFACTURING THEM

Abstract

The present disclosure relates generally to carbon-based products. More particularly, the present disclosure relates to acid-impregnated carbon-based products having at least one nitrogen- containing compound covalently bound to a porous carbon matrix, methods of making same, and uses of same in industry and agriculture.

Description

1 / 54 CARBON-BASED PRODUCTS AND METHODS OF MANUFACTURING THEM TECHNICAL FIELD

[0001] The present disclosure relates generally to carbon-based products. More particularly, the present disclosure relates to acid-impregnated carbon-based products having at least one nitrogen-containing compound covalently bonded to a porous carbon matrix, methods of manufacturing the same, and uses thereof in industry and agriculture. FUNDAMENTALS

[0002] Agriculture today is defined by the need for massive increases in crop productivity through accelerated modernization to support the growing global human population while minimizing negative environmental impacts. However, soil nutrients are often not being replenished efficiently to sustainably maintain high crop yields or are being lost through leaching and volatilization, resulting in economic losses for farmers due to the need for reapplication and over-application of fertilizers. Many common fertilizers that exist today are applied in highly water-soluble forms, making them susceptible to leaching and / or volatilization, which has both economic and environmental costs.The global problem of fertilizer runoff is growing and being exacerbated by population growth, urbanization, and the consequent constant need for ever-increasing agricultural yields.

[0003] The inefficient use of nitrogen (N) fertilizers has been a major concern in agriculture. Nitrogen use efficiency, defined as the percentage of N applied to the crop, for cereal crops varies between 21-41%, with a global average of 35% (Omara et al., 2019) and is based on the type of fertilizer used, application method, time, rate of Petition 870250099571, dated 10 / 30 / 2025, page 9 / 69 2 / 54 Application and Environment. The main pathways of N loss are nitrate leaching and gaseous loss via ammonia volatilization. N loss through ammonia volatilization increases with soil pH, temperature, and application method. Higher temperatures increase urease activity, and surface application facilitates ammonia diffusion into the atmosphere. Loss can be greater than 15%, regardless of environmental and soil conditions. In warmer climates, N loss from urea application reaches 78% (global demand in 2020 was 118.7 million tons of urea fertilizer, while nitrogen use efficiency was only 38%). In certain cases, farmers will still use surface urea application, resulting in greater nitrogen loss through ammonia volatilization.Furthermore, enhanced efficiency fertilizers have been identified as an essential component of 4R nutrient management to help mitigate nitrogen losses from synthetic fertilizers. These fertilizers have demonstrated reductions in ammonia volatilization, leaching losses that are harmful to aquatic environments, and potent greenhouse gases in the form of nitrous oxide emissions, all while maintaining or improving crop yields. 4R nutrient management is recommended for the use of fertilizers at the right rate, at the right time, from the right source, and in the right place to minimize losses and increase nutrient use efficiency, which will eventually be useful for increasing agricultural production and farmer profit. However, it is not always possible to follow the 4R principles for all farmers due to management and logistics issues, equipment limitations, or access to fertilizer technologies.Therefore, it is essential to identify the best management practice to meet the interests of farmers, which is always challenging, as certain practices do not work well everywhere and in every situation. Therefore, innovation is key. Petition 870250099571, dated 10 / 30 / 2025, page 10 / 69 3 / 54 New technologies that can fill these gaps have a tremendous opportunity to help meet farmers' interests in increasing crop productivity and return on investment, while adapting to common and economical application methods.

[0004] Carbon-based fertilizers, also known as organomineral fertilizers, have demonstrated multiple benefits in the agricultural industry, such as increased soil fertility and quality (Hertsgaard, 2014). Carbon-based fertilizers can also mitigate the negative impacts of heavy metals and other pollutants in the soil (Hertsgaard, 2014). Carbon-based fertilizers have a highly porous structure and can have large surface areas. In the soil, these attributes allow for the adsorption and potential slow release of nutrients, the adsorption of dissolved organic compounds, and provide a space for microorganisms and fungi to reside. This can contribute to significant improvements in overall soil health through increased soil fertility, improved soil structure, and enhanced soil chemistry and biology.Furthermore, if carbon-based fertilizer is processed in a way that creates properties that resist decomposition, the source materials can be diverted from a source of greenhouse gases (GHG) to a potential sink when placed in the soil due to the slow degradation of the carbon material (Spear, 2018).

[0005] However, carbon-based fertilizers are not common due to the high temperatures required to produce them, low nutrient content, low density, handling difficulties, low yield, and there is a need in the art for carbon-based products that are produced at lower temperatures with higher nutrient contents and better fertilizer properties, such as greater retention and Petition 870250099571, dated 10 / 30 / 2025, page 11 / 69 4 / 54 Slow release of nitrogen-containing compounds. BRIEF SUMMARY

[0006] In a first aspect of the present disclosure, a method for producing a porous carbon matrix product from a carbonaceous biomass material is provided. The method comprises: (a) treat the carbonaceous biomass material with at least one nitrogen-containing compound; (b) applying a mineral acid to the carbonaceous biomass material while mixing both components for a period of time, thereby leaving the mineral acid impregnated in the carbonaceous biomass material and covalently linking the nitrogen-containing compound to the carbonaceous biomass material; and (c) converting the mineral acid into its corresponding salt by exposing the acid-impregnated carbonaceous biomass material to ammonia, wherein the porous carbon matrix product contains nitrogen bound to the porous carbon matrix.

[0007] In one embodiment of the method provided in this document, step (b) is performed before step (a).

[0008] In one embodiment of the method provided in this document, the covalently bonded nitrogen is from the nitrogen-containing compound and / or the salt.

[0009] In one embodiment of the method provided in this document, carbonaceous biomass material comprises wood, digested, composted or raw animal manure, lignocellulosic materials, agricultural residues, agricultural by-products, organic residues, organic by-products, peat, bagasse, palm oil residues, palm oil by-products, straw, municipal solid waste, bedding materials containing manure, food residues and by-products, nut shells or coconut fiber.

[0010] In one embodiment of the method provided in this document, Petition 870250099571, dated 10 / 30 / 2025, page 12 / 69 5 / 54 Carbonaceous biomass material comprises wood, and wood comprises wood chips, wood pulp or wood powder.

[0011] In one embodiment of the method provided in this document, the carbonaceous biomass material comprises wood, and the wood is pine wood.

[0012] In one embodiment of the method provided in this document, at least one nitrogen-containing compound is present in an aqueous solution.

[0013] In one embodiment of the method provided in this document, at least one nitrogen-containing compound has an active or available carbonyl or imine group.

[0014] In one embodiment of the method provided in this document, at least one nitrogen-containing compound comprises an active or available carbonyl or imine group.

[0015] In one embodiment of the method provided in this document, at least one nitrogen-containing compound comprises urea.

[0016] In one embodiment of the method provided in this document, at least one nitrogen-containing compound comprises urea in an amount to achieve a specified nutrient profile.

[0017] In one embodiment of the method provided in this document, step (b) further comprises the application of heat, in addition to the application of the mineral acid.

[0018] In one embodiment of the method provided here, the The temperature of step (b) does not exceed 400 degrees Celsius, preferably does not exceed 350 degrees Celsius, more preferably does not exceed 300 degrees Celsius, more preferably does not exceed 250 degrees Celsius, more preferably does not exceed 200 degrees Celsius, more preferably does not exceed 150 degrees Celsius and more preferably does not exceed 100 degrees Celsius.

[0019] In one embodiment of the method provided in this document, the mineral acid is sulfuric acid, nitric acid, phosphoric acid, polyphosphoric acid, hydrochloric acid and / or a combination of Petition 870250099571, dated 10 / 30 / 2025, page 13 / 69 6 / 54 same.

[0020] In one embodiment of the method provided in this document, the mineral acid is sulfuric acid.

[0021] In one embodiment of the method provided in this document, ammonia is ammonia gas or aqueous ammonia.

[0022] In one embodiment of the method provided in this document, step (c) comprises flowing an ammonia gas or aqueous ammonia over or through the acid-impregnated carbonaceous biomass material.

[0023] In one embodiment of the method provided in this document, the salt is ammonium sulfate, ammonium nitrate, ammonium phosphate, or ammonium chloride.

[0024] In one embodiment of the method provided in this document, the salt is ammonium sulfate.

[0025] In one embodiment of the method provided in this document, the method further comprises, before carrying out steps (a), (b) and (c), grinding the carbonaceous biomass material to a suitable particle size range.

[0026] In one embodiment of the method provided in this document, the method further comprises, after step (c), sieving, pelletizing or granulating the porous carbon matrix product into a suitable particle size range.

[0027] In a second aspect of the present disclosure, a porous carbon matrix product is provided. The porous carbon matrix product is produced by the method according to the first aspect.

[0028] In one embodiment of the porous carbon matrix product provided in this document, ammonia volatilization is reduced, compared with the product produced without treating the carbonaceous biomass material with at least one nitrogen-containing compound.

[0029] In one embodiment of the porous carbon matrix product provided in this document, the release nitrogen Petition 870250099571, dated 10 / 30 / 2025, page 14 / 69 7 / 54 is slow-moving inorganic nitrogen.

[0030] In one embodiment of the porous carbon matrix product provided in this document, the slow-release nitrogen is organic nitrogen.

[0031] In a third aspect of the present disclosure, a slow-release fertilizer product is provided. The slow-release fertilizer product comprises a porous carbon matrix and at least one nitrogen-containing compound covalently bonded to the porous carbon matrix, wherein the porous carbon matrix is ​​impregnated with an ammonium mineral acid salt.

[0032] In one embodiment of the slow-release fertilizer product provided in this document, at least one nitrogen-containing compound comprises an active or available carbonyl or imine group.

[0033] In one embodiment of the slow-release fertilizer product provided in this document, at least one nitrogen-containing compound comprises urea.

[0034] In one embodiment of the slow-release fertilizer product provided in this document, the mineral acid is sulfuric acid, nitric acid, phosphoric acid, polyphosphoric acid, hydrochloric acid and / or a combination thereof.

[0035] In one embodiment of the slow-release fertilizer product provided in this document, at least one nitrogen-containing compound is released from the fertilizer due to microbial activity over the course of a growing season.

[0036] In one embodiment of the slow-release fertilizer product provided in this document, ammonia volatilization is reduced, compared with the product produced without treating the carbonaceous biomass material with at least one nitrogen-containing compound.

[0037] In one embodiment of the slow-release fertilizer product provided in this document, the slow-release nitrogen is inorganic nitrogen. Petition 870250099571, dated 10 / 30 / 2025, page 15 / 69 8 / 54

[0038] In one embodiment of the slow-release fertilizer product provided in this document, the slow-release nitrogen is organic nitrogen. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] So that the subject matter of this revelation may be easily understood, the modalities are illustrated by means of the attached drawings.

[0040] Figure 1 is an image of pine wood chips, a carbonaceous biomass material used as a starting material for certain embodiments of the invention.

[0041] Figure 2 shows images of carbonaceous biomass material before and after acidification with sulfuric acid.

[0042] Figure 3 shows images of acidified carbonaceous biomass material during the ammoniation process using aqueous ammonia solution.

[0043] Figure 4 is a graph illustrating the cumulative loss of ammonia volatilization from urea and porous carbon matrix products treated with urea before and after acidification.

[0044] Figure 5 is a graph illustrating the cumulative loss of ammonia volatilization from urea and porous carbon matrix products treated with urea before acidification and added temperature during acidification.

[0045] Figure 6 is a graph illustrating the cumulative loss of ammonia volatilization from urea and porous carbon matrix products treated with urea before acidulation with the addition of temperature or ambient conditions during acidulation.

[0046] Figure 7 is a graph illustrating the recovered N as a % of the total N applied for ammonium sulfate, urea and environmentally smart nitrogen fertilizers, and various porous carbon matrix products treated with urea prior to acidulation, and various acidulation reaction temperatures.

[0047] Other features and advantages of the present disclosure will become clearer from the following description. Petition 870250099571, dated 10 / 30 / 2025, page 16 / 69 9 / 54 detailed and exemplary modalities. DETAILED DESCRIPTION DEFINITIONS

[0048] The terminology used in this document is intended to describe only particular embodiments and is not intended to be limiting of exemplary embodiments of the invention. Unless otherwise defined, all technical and scientific terms used in this document generally have the same meaning as commonly understood by those ordinarily skilled in the art. Generally, nomenclatures used in connection with the methods described in this document are those well known and commonly used in the art. However, definitions of selected terms are provided below for greater clarity and consistency.

[0049] As used in this document, the singular forms after “a / an” and “the” should also include the plural forms, unless the context clearly indicates otherwise.

[0050] The phrase “and / or” should be understood as meaning “one or both of the elements thus conjugated,” that is, elements that are conjuncturally present in some cases and disjuncturally present in other cases. Thus, as a non-limiting example, a reference to “A and / or B,” when used in conjunction with open language such as “including,” may refer, in one modality, only to A (optionally including elements other than B); in another modality, only to B (optionally including elements other than A); in yet another modality, to both A and B (optionally including other elements); etc.

[0051] As used in this document, the phrase “one or more,” in reference to a list of one or more elements, should be understood as meaning at least one element selected from any one or more elements in the list of elements, but not necessarily including at least one of each element. Petition 870250099571, dated 10 / 30 / 2025, p. 17 / 6910 / 54 specifically listed within the list of elements and not excluding any combinations of elements in the list of elements. This definition also allows elements to optionally be present in addition to the elements specifically identified within the list of elements to which the phrase "one or more" refers, whether or not they are related to those specifically identified elements.Thus, as a non-limiting example, “one or more of A and B” (or, equivalently, “one or more of A or B”, or, equivalently “one or more of A and / or B”) may refer, in one embodiment, to at least one, optionally including more than one, A, without B present (and optionally including elements other than B); in another embodiment, to at least one, optionally including more than one, B, without A present (and optionally including elements other than A); in yet another embodiment, to at least one, optionally including more than one, A, and at least one, optionally including more than one, B (and optionally including other elements); etc.

[0052] When the term “about” is used in conjunction with a numerical range, it modifies that range by extending the limits above and below those numerical values. In general, the term “about” is used here to modify a numerical value above and below the stated value by a variation of 20%, 10%, 5%, or 1%. In certain embodiments, the term “about” is used to modify a numerical value above and below the stated value by a variation of 10%. In certain embodiments, the term “about” is used to modify a numerical value above and below the stated value by a variation of 5%. In certain embodiments, the term “about” is used to modify a numerical value above and below the stated value by a variation of 1%.

[0053] When a range of values ​​is listed here, the intention is to cover every value and subrange within that range. For example, “1-5 g” is intended to cover 1 g, 2 g, 3 g, Petition 870250099571, dated 10 / 30 / 2025, page 18 / 69 11 / 54 g, 5 g, 1-2 g, 1-3 g, 1-4 g, 1-5 g, 2-3 g, 2-4 g, 2-5 g, 3-4 g, 3-5 g and 4-5 g.

[0054] It should also be understood that the terms comprise, “comprising”, “includes” and / or “including”, when used in this document, specify the presence of declared features, integers, steps, operations, elements and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components and / or groups thereof.

[0055] The term “consisting of” and its derivatives, as used in this document, are intended to be closed terms that specify the presence of declared features, integers, steps, operations, elements and / or components and exclude the presence or addition of one or more other features, integers, steps, operations, elements and / or components.

[0056] “Carbonaceous material means any biomass material, which includes living or formerly living biological material, such as plants, animals, algae or microorganisms, or any materials or residues formed from organisms that once lived. Carbonaceous materials may include, without limitation, textile waste, marine waste, wood and other lignocellulosic material, agricultural waste or by-products, organic waste, organic by-products, animal waste or by-products such as digested or composted animal manure, agricultural by-products such as raw, digested or composted animal manure, peat, bagasse, palm oil by-products or residues, straw, compost or municipal solid waste, bedding materials containing manure, food waste, by-products or residues of food production, nut shells, coconut fiber and fossil fuels and by-products of fossil fuels such as coal and petroleum coke.The terms “carbonaceous material,” “carbonaceous biomass material,” and... Petition 870250099571, dated 10 / 30 / 2025, page 19 / 69 12 / 54 biomass are used interchangeably in this document.

[0057] Mineral acid means any inorganic acid, including, but not limited to, sulfuric, phosphoric, polyphosphoric, nitric or hydrochloric acid and / or combinations thereof.

[0058] The terms porous carbon and porous carbon matrix are used interchangeably and mean a solid microporous material produced at temperatures below pyrolysis temperatures, with a high surface area in a solid form, consisting of stable and labile forms of carbon, sufficiently porous to allow the passage of gas into its internal spaces. Composed mainly of carbon, oxygen and hydrogen and containing small amounts of other elements originally found in the carbonaceous materials from which the porous carbon was formed, which may include, but are not limited to, elements such as nitrogen, sulfur, phosphorus, silicon, aluminum, iron, calcium, magnesium, sodium and potassium.

[0059] Gas means any substance or combination of substances that exists in a gaseous state at standard temperature and pressure.

[0060] Chemisorption means the attachment or adsorption of a gas molecule onto a solid or liquid surface and any reactions that may occur between the gas molecule and the solid or liquid.

[0061] Acidulation, as used in this document, refers to a process in which a sample of carbonaceous biomass is impregnated with acid, such as, but not limited to, sulfuric acid (SA), phosphoric acid (PA), nitric acid (NA), hydrochloric acid (HCl) or polyphosphoric acid (PPA).

[0062] Ammoniation, as used in this document, refers to a process in which a sample is treated with ammonia gas (NH3) or liquid ammonia (e.g., aqueous ammonia solution) to neutralize residual acid or react with surface portions on the carbon matrix surface. Petition 870250099571, dated 10 / 30 / 2025, page 20 / 69 13 / 54

[0063] Carbonization, as used in this document, refers to a process of dehydrating a sample, resulting in a porous carbon matrix.

[0064] Slow-release fertilizer, as used in this document, refers to the release of the desired nutrient in a fertilizer, such as, but not limited to, nitrogen, sulfur, or potassium, at a desired release rate in the soil, which minimizes the loss of the nutrient to the surrounding environment, making it unavailable for plant uptake. The criteria for the release rate may depend on the type of nutrient. For example, with nitrogen, the criteria for a slow-release fertilizer may require that there be at least 15% of N in a slowly available form when compared to a soluble reference product (AAPFCO, 2011). Other criteria may require that no more than 15% of nutrients be released in 24 hours; no more than 75% released in 28 days; and at least approximately 75% released at the stated release time.

[0065] Enhanced Efficiency”, as used in this document, refers to fertilizer products with characteristics that allow for greater availability of nutrients to plants and reduce the potential for nutrient losses to the environment when compared to an appropriate reference product (AAPFCO, 2009).

[0066] The terms “nitrogen treatment”, “nitrogen pretreatment” and “pretreatment” are used interchangeably in this document to refer to the addition of a nitrogen-containing compound to a carbonaceous biomass material, before or after acidification with a mineral acid.

[0067] The terms “Nitro CCT” and “N-treated CCT” and “CCT” are used interchangeably in this document to refer to the final carbon product having the carbonaceous material treated with a nitrogen-containing compound before or after acidulation with a mineral acid, treated with a mineral acid, followed by Petition 870250099571, dated 10 / 30 / 2025, page 21 / 69 14 / 54 treatment with an ammonia source to neutralize any remaining residual acid. GENERAL METHODS

[0068] The inventors previously discovered that carbonaceous materials react with liquid acid to form a porous carbon matrix impregnated with the acid. This reaction can occur under ambient conditions, as described in U.S. Patent 8,198,211, which is incorporated herein by reference.

[0069] In general terms, a porous carbon matrix impregnated with acid can be formed by: 1. If necessary, adjust the moisture content of a carbonaceous material to the desired level; 2. Adjust the particle size of the carbonaceous material to the desired range; 3. Apply liquid acid to the carbonaceous material; and 4. Mix the carbonaceous material and the liquid acid until the chemical reaction is complete.

[0070] Carbonaceous material may comprise any suitable biomass material, including wood and other lignocellulosic materials, agricultural residues, agricultural by-products, organic residues, organic by-products, animal residues or by-products such as raw, digested or composted animal manure, peat, bagasse, palm oil residues, palm oil by-products, straw, municipal solid waste, bedding materials containing manure, nut shells, coconut fiber, coal and petroleum coke. Wood chips or shavings are a particularly preferred carbonaceous material.

[0071] The moisture content of carbonaceous material depends on the raw material and particle size and can range from about zero to 50% on a wet mass basis, preferably about 5 to 35%. Carbonaceous material can be dried if the moisture content is higher than the desired level, or water can be Petition 870250099571, dated 10 / 30 / 2025, page 22 / 69 15 / 54 added to the carbonaceous material to increase the moisture content to the desired level.

[0072] Carbonaceous material can be processed into particles of an appropriate size, depending on the intended application and the raw material, by any suitable method, including, for example, chopping, grinding, cutting or otherwise reducing the particle size. Furthermore, if the raw material consists of very small particles, the particles can be agglomerated to create larger particles of a suitable size. The particle size of the carbonaceous material can have an average range of about 0.1 mm to 10 mm, preferably about 0.1 to 5 mm, and more preferably about 0.1 to 1 mm.

[0073] The liquid acid used for acidification can be any suitable mineral acid, such as sulfuric, phosphoric, polyphosphoric, hydrochloric or nitric acid and / or combinations thereof. The choice of acid will change the salt formed if the acid reacts with a chemisorbed molecule. Therefore, if ammonia is used, then the use of sulfuric acid will result in the formation of ammonium sulfate.

[0074] The concentration of liquid acid used depends on the moisture content of the carbonaceous material and the desired nutrient content of the final carbon-based product. Suitable acid concentrations may range from about 20 to 100%, preferably about 75 to 100%, and more preferably 100% (where 100% is the concentrated form of the acid). The amount of liquid acid used depends in part on the desired nutrient analysis and may range from a ratio of about 0.20:1 acid:biomass to 2.5:1 acid:biomass (by weight).

[0075] The carbonaceous material and the liquid acid are mixed until the reaction is substantially complete. The time period depends on the moisture content, particle size, acid concentration, and raw material:acid ratio, but is usually between about 2 and 35 minutes, preferably Petition 870250099571, dated 10 / 30 / 2025, p. 23 / 69 16 / 54 between approximately 5 to 25 minutes, and more preferably between approximately 15 minutes.

[0076] In one embodiment, the completion of the reaction can be monitored by temperature. As the reaction begins, the temperature typically rises until it reaches a maximum and falls as the reaction is completed.

[0077] In one embodiment, liquid acid is sprayed onto the carbonaceous material as mixing progresses. In another embodiment, the carbonaceous material is formed into pellets, and then liquid acid is applied to the pelletized form of the carbonaceous material.

[0078] In one embodiment, the conversion of the carbonaceous material into a porous carbon matrix and the acid impregnation occur in a single step. Furthermore, the acid-impregnated porous carbon matrix does not require additional processing before use as a chemisorbent.

[0079] In one embodiment, the porous carbon matrix can be used to remove ammonia from a gas stream. The ammonia reacts with inorganic acids to form the corresponding ammonium salt and will be retained by the solid porous carbon matrix as the gas or liquid passes through.

[0080] A stream of gas or liquid containing ammonia may be routed through a reaction vessel comprising the acid-impregnated porous carbon matrix, in solid, granular or pelletized form. The porous carbon matrix may comprise a fixed bed or may be disturbed by the gas flow or by mechanical means, such as with a fluidized bed, drum granulator or pseudofluidized bed. Preferably, means are provided for periodically replenishing or replacing the porous carbon matrix.

[0081] Ammonia is chemisorbed by the acid-impregnated porous carbon matrix and converted into a fertilizer salt with little residual acidity and containing carbon, oxygen, hydrogen and Petition 870250099571, dated 10 / 30 / 2025, page 24 / 69 17 / 54 other elements. In this way, the spent porous carbon matrix is ​​a useful source of selected nutrients for agricultural and horticultural applications. In this way, the cost of ammonia removal is reduced and a value-added byproduct is created.

[0082] The porous carbon matrix product can be pelletized or granulated using conventional methods to form fertilizer pellets or otherwise processed into a useful agricultural or horticultural form.

[0083] The inventors discovered that treating carbonaceous material with at least one nitrogen-containing compound before or after applying liquid acid to the carbonaceous material can produce carbon-based fertilizers with a higher nitrogen content. Suitable nitrogen-containing compounds contain an activated carbonyl group, for example, in urea (carbamide), or an imine group, for example, in arginine. Furthermore, the inventors discovered that treating carbonaceous material with at least one nitrogen-containing compound before applying liquid acid to the carbonaceous material and adding heat below 350 °C during the liquid acid treatment of the carbonaceous material can produce carbon-based fertilizers with a slow-release mechanism of nitrogen compounds and a decrease in the ammonia volatilization potential.

[0084] Carbonaceous material can be treated with a nitrogen-containing substance before or after acidification. The amount of nitrogen used during treatment depends in part on the desired nutrient retention and nutrient analysis. Suitable nitrogen treatment concentrations can range from about 2:1 treatment:biomass to about 1:5 treatment:biomass (by dry weight). Nitrogen treatments are typically dissolved with minimal water and added to the carbonaceous material, allowing them to penetrate the biomass material. Suitable acid concentrations can Petition 870250099571, dated 10 / 30 / 2025, page 25 / 69 18 / 54 vary from about 0.20:1 acid:biomass to about 2:1 acid:biomass (by weight). Suitable heat treatments may be lower than pyrolysis temperatures and may include temperatures below 400 °C, preferably below 350 °C, more preferably below 300 °C, more preferably below 250 °C, more preferably below 200 °C, more preferably below 150 °C, and more preferably below 100 °C. Suitable heat treatments may have a range of 100 °C to 350 °C during acidification and, more preferably, below about 200 °C. The desired potential for slow release or reduction of ammonia volatilization depends, in part, on the amount of liquid acid used during the treatment of the carbonaceous material and the temperature applied during the acidification of the carbonaceous material.With high acid ratios and high temperature, carbonaceous material will degrade at a higher rate compared to a high acid ratio and lower temperature or a low acid ratio and lower temperature. EXAMPLES

[0085] The revelation is described in more detail by reference to the following examples. These examples are provided for illustrative purposes only and are not intended to be limiting unless otherwise specified. Thus, the revelation should in no way be interpreted as limited to the following examples, but rather should be interpreted to encompass any and all variations that become evident as a result of the teaching provided in this document. EXAMPLE 1: Development of Pretreatment Methods for Carbonaceous Biomass Materials

[0086] Several methods for pretreating a sample of carbonaceous biomass (e.g., wood chips) were examined to investigate the potential nitrogen retention in the carbon matrix and the slow-release qualities of Petition 870250099571, dated 10 / 30 / 2025, page 26 / 69 19 / 54 nitrogen from carbon samples.

[0087] A carbonaceous biomass material consisting of pine wood chips (Figure 1) was pretreated with different sources of nitrogen and phosphate to determine if such modifications to the biomass affect nutrient retention in the resulting porous carbon matrix product. Combustion analysis was used to measure the percentages of total sulfur (TS), total carbon (TC), and total nitrogen (TN) in the pretreated and acidified sample, the ammoniated sample, and the washed ammoniated sample to determine if there was any nutrient retention in the resulting porous carbon matrix product. An additional ion chromatography method was used to measure the percentage of N washed from the product. Materials and methods:

[0088] The following general process was used to produce the porous carbon matrix with retained nitrogen product: 1. Pretreatment: A nitrogen source contained in an aqueous solution or in a gas (i.e., ammonia gas) was added to the carbonaceous material at a specific ratio of nitrogen source to biomass based on dry weight. The nitrogen source solution was soaked with the biomass for a certain period of time, followed by optional overnight drying of the biomass at 70 °C before the acidification step. 2. Acidulation: A mineral acid (i.e., sulfuric acid) was slowly added to the pre-treated carbonaceous material (i.e., pine wood chips) at a ratio of 1:1 acid to pre-treated biomass based on dry weight. The resulting acidified porous carbon matrix sample was slowly stirred manually with a glass rod for 5 minutes or until all the carbonaceous biomass was coated / reacted. The highest temperature of the acidulation reaction was recorded. The samples were then partitioned for combustion analysis. The samples were dried at 70 °C for Petition 870250099571, dated 10 / 30 / 2025, p. 27 / 69 20 / 54 the night before combustion analysis. 3. Ammoniation: Pretreated and acidified porous carbon matrix samples were placed in an ammonia atmosphere within a sealed vacuum chamber. The lid was properly lubricated, and a tight seal was ensured before use of the vacuum chamber. The samples were evenly distributed in the chamber and then aerated with gaseous ammonia in the sealed chamber for 2 hours. To ensure uniform ammoniation treatment, the samples were periodically mixed in the vacuum chamber, and the process was repeated if necessary. After ammoniation was completed by the total neutralization test, the samples were vacuum filtered before being dried in an oven at 70 °C or until the moisture content was less than 5%. The samples were weighed and then partitioned for combustion analysis. 4. Alternative Ammonization Procedure: Pre-treated and acidified porous carbon matrix samples were slowly added to the aqueous ammonia solution and manually stirred with a glass rod for 5 minutes or until all pine wood chips were coated / reacted to neutralize residual acid. The highest temperature of the ammonization reaction was recorded. The samples were then partitioned for combustion analysis. The samples were dried at 70 °C overnight before combustion analysis. 5. Washing Procedure: Pre-treated, acidified, and ammoniated porous carbon matrix (CCT) samples were extracted using deionized water, unless otherwise indicated. Samples were stirred for 1 hour before decantation. The process was monitored by pH and electrical conductivity (EC) to ensure that the samples were thoroughly washed to remove any soluble salts or residual acid. Samples were then vacuum filtered using filter paper and dried. Petition 870250099571, dated 10 / 30 / 2025, page 28 / 69 21 / 54 oven at 70 °C and weighed before combustion analysis to measure retained nutrients. 6. Alternative Washing Procedure: Pre-treated, acidified, and ammoniated porous carbon matrix (CCT) samples were extracted with deionized water (DI) using the Standard Operating Procedure (SOP) for Extraction of Available N from Soil Samples (Maynard and Karla, 1993), as set out below.

[0089] In a 50 mL centrifuge tube, 5 g of sample were weighed and 25 mL of DI water were added. The tubes were shaken in a soil shaker for 1 hour to ensure good extraction. After shaking, the tubes were centrifuged at 4000 rpm for 5 minutes to allow sedimentation of the solids. The samples were then decanted, filtered through a 0.45 μm filter, and the collected filtrates were analyzed using ion chromatography (IC) for ammonium, nitrate, and nitrite, as well as soluble organic N (i.e., urea) using combustion analysis or, when indicated, the persulfate method (Borba et al., 2016) followed by IC analysis. The nitrogen content in the filtrate was then calculated to determine the amount of nitrogen removed from the CCT sample. The amount retained and not removed from washing was calculated as a % of C bound to N. Results:

[0090] In an initial analysis, three types of carbonaceous biomass materials—fine wood sawdust, pine wood chips, and soluble seaweed extracts—were used to produce porous carbon matrix products without any nitrogen pretreatment. Combustion analysis of TC, TN, and TS revealed that the three biomass types were comparable, as shown in Table 1. Furthermore, after ammoniation and washing, no nitrogen was retained in the sample. Table 1: Results of combustion analysis of various Petition 870250099571, dated 10 / 30 / 2025, page 29 / 69 22 / 54 carbonaceous biomass materials (fine wood sawdust, pine wood shavings and soluble seaweed extract) after acidification, ammoniation and washing. (*) indicates that the sample exceeded the calibration range. Biomass Combustion Analysis (%) TC TN TS Fine Wood Sawdust 45 0.4 <0.06 Acidulated Fine Wood Sawdust 23 0.28 14* Acidulated and Ammoniated Fine Wood Sawdust - Washed 46 0.4 0.81 Pine Wood Chips 44 0.4 <0.06 Acidulated Pine Wood Chips 19 0.22 15 Acidulated and Ammoniated Pine Wood Chips - Washed 54 0.5 0.96 Soluble Seaweed Extract 26 0.6 1.2 Acidulated Soluble Seaweed Extract 24 0.49 16* Acidulated and Ammoniated Soluble Seaweed Extract - Washed 48 1.6 0.38

[0091] The following pretreatment methods were then evaluated: • No chemical pretreatment (i.e., pretreatment was limited to physical treatments to achieve a target moisture content and appropriate particle size) (No Pretreatment); • Pre-treatment of biomass with aqueous ammonia (Aq. Ammonia) at a 1:1 ratio of aqueous ammonia:biomass for 30 minutes, followed by overnight drying at 70 °C (Aq. Ammonia Pre-treatment); • Pre-treatment of biomass with gaseous ammonia in a sealed and pressurized container for 1-2 hours; • Pre-treatment of biomass with a lysine solution Petition 870250099571, dated 10 / 30 / 2025, page 30 / 69 23 / 54 in a 0.6:1 lysine:biomass ratio followed by overnight drying at 70 °C; • Pre-treatment of biomass with an arginine solution at a ratio of 0.6:1 arginine:biomass followed by overnight drying at 70 °C; (Arginine Pre-treatment); • Pre-treatment of biomass with ammonium polyphosphate (APP) solution at a 2:1 ratio of APP solution to biomass overnight, followed by overnight drying at 70 °C (APP Pre-treatment).

[0092] When monitoring the acidulation reaction after biomass pretreatment, the highest reaction temperatures (i.e., highest exotherms) reached are shown in Table 2. The highest reaction temperature reached by the arginine and aqueous ammonia pretreatments was 125 °C and 153 °C, respectively, compared to a peak temperature of 85 °C for the APP treatment. Table 2: The reaction temperature of the acidified porous carbon matrix and the pH and EC (electrical conductivity) of the filtrate after washing with DI water. Sample Acidification Filtrate Temperature (°C) pH EC (pS / cm) Without Pretreatment 150 7.19 330.5 Pretreatment with APP 85 7.94 5.8 Pretreatment with Arginine 125 7.27 400.1 Pretreatment with Aqueous Ammonia 153 7.36 407.4

[0093] Pretreated samples of biomass (i.e., pine wood chips) were then acidified, ammoniated, washed, and at each step analyzed by combustion analysis to determine the effect of pretreatment on the acidification reaction and the final nutrient analysis (Table 3). Petition 870250099571, dated 10 / 30 / 2025, page 31 / 69 24 / 54

[0094] Among the pretreatments analyzed, arginine showed the highest N retention after ammoniation and washing of the ammoniated material (Table 3). This indicates that there was some chemical bonding of nutrients to the carbon matrix due to some functional moieties. Other pretreatments, such as with APP or aqueous ammonia (also referred to as aq. ammonia), showed very little nitrogen retention in the carbon matrix after ammoniation and washing of the ammoniated material. Table 3: Results of the combustion analysis of acidified, ammoniated and washed pine wood chips, pre-treated with APP, arginine and aqueous ammonia. Sample Combustion Analysis (%) TC TN TS Pretreatment with APP 11 4.1 15 Pretreatment with APP - Washed 46 1.3 1.7 Pretreatment with Arginine 18 5.5 16 Pretreatment with Arginine - Washed 45 6.2 2.9 Pretreatment with Aqueous Ammonia 21 0.34 16 Pretreatment with Pretreatment with Ammonia Washed 53 0.5 0.93

[0095] In summary, these tests showed that porous carbon matrix products pretreated with arginine exhibited the highest total nitrogen retention among the pretreatments tested. EXAMPLE 2: Optimization of Carbonaceous Biomass Pretreatment Methods

[0096] Experiments were conducted to better investigate whether different nitrogen sources at different concentrations affect the nutrient retention of the resulting porous carbon matrix (CCT) product. Pre-treatment: Petition 870250099571, dated 10 / 30 / 2025, page 32 / 69 25 / 54

[0097] Pretreatments were prepared in a beaker and then slowly added to a 50 g sample of carbonaceous biomass, i.e., pine wood chips. A glass rod was used to stir the sample to ensure that all pine wood chips were uniformly mixed with the pretreatment solution. The standard immersion time at room temperature for all pretreatments was 3 days, unless otherwise specified. Pretreated samples were then dried overnight at 70 °C before acidification.

[0098] Urea solutions were tested as a pretreatment for carbonaceous biomass samples. For the pretreatment, 50 g of pine wood chips were soaked in urea:biomass ratios of 0.3:1, 0.6:1, and 1:1 based on dry weight. The soaking times for urea:biomass pretreatments at a 0.6:1 ratio were: (a) 1 day; (b) 3 days (standard soaking time); (c) 1 week; and (d) 4 weeks. The soaking times for urea:biomass pretreatments at a 1:1 ratio were: (a) 1 day; and (b) 3 days (standard soaking time). The pretreated samples were placed in a vacuum chamber for 5 hours, then dried overnight at 70 °C before acidification.

[0099] Arginine solutions were tested as a pretreatment for carbonaceous biomass samples at arginine:biomass ratios of 0.3:1 and 0.6:1 based on dry weight. For the pretreatment, 50 g of pine wood chips were soaked in the respective arginine solutions for 1 day, then dried overnight at 70 °C before acidification.

[00100] Lysine solutions were tested as a pretreatment for carbonaceous biomass samples at lysine:biomass ratios of 0.3:1, 0.6:1 and 1:1 based on dry weight. For the pretreatment, 50 g of pine wood chips were soaked in the respective lysine solution for 1 day and then dried overnight at 70 °C before acidification.

[00101] Aqueous ammonia (30% by weight NH3 solution in water) Petition 870250099571, dated 10 / 30 / 2025, page 33 / 69 26 / 54 was tested as a pretreatment for carbonaceous biomass samples. For the pretreatment, 50 g of pine wood chips were soaked in the respective concentration at a 1:1 ratio of aqueous ammonia:biomass (by weight). Additionally, biomass samples overloaded with aqueous ammonia were also tested. For the overload pretreatments, pine wood chips were treated with aqueous ammonia, dried, and treated again twice more at a 1:1 ratio of aqueous ammonia:biomass (by weight) with drying between treatments to maximum saturation (i.e., for a total of three consecutive pretreatments with aqueous ammonia).

[00102] Polyacrylamide solution was tested as a pretreatment for carbonaceous biomass samples at a 0.3:1 polyacrylamide:biomass ratio based on dry weight. Due to the gelling nature of polyacrylamide, only the 0.3:1 ratio was investigated. Acidulation:

[00103] Sulfuric acid was slowly added to pretreated pine wood chips at a 1:1 ratio of sulfuric acid to pretreated biomass. The resulting acidified porous carbon matrix sample was slowly stirred manually with a glass rod for 5 minutes or until all the pine wood chips were coated / reacted. The highest temperature of the acidification reaction was recorded.

[00104] The samples were then partitioned for analysis via combustion analysis. The samples were dried at 70 °C before combustion analysis. Ammonization:

[00105] Several acidulated and pretreated porous carbon matrix samples were subsampled to be ammoniated with aqueous ammonia at a 1:1 ratio of aqueous ammonia solution to acidulated biomass (Figure 3). To ensure uniform ammoniation treatment, the samples were periodically mixed in the container for a period of three days. The Petition 870250099571, dated 10 / 30 / 2025, page 34 / 69 27 / 54 of the following samples were ammoniated: Pre-treated and acidified urea (0.3:1, 0.6:1 ratios) Pre-treated and acidified arginine (ratios of 0.3:1, 0.6:1) Aqueous ammonia (1:1, overload) pre-treated and acidified Washing:

[00106] All samples were washed by vacuum filtration and monitored for pH and EC. The samples were then oven-dried at 70 °C overnight. The samples were weighed and then partitioned for combustion analysis to measure retained nutrients.

[00107] Available / exchangeable nitrogen (including ammonium, nitrate, and nitrite) in the samples was extracted with DI water, 2 M KCl, and 0.5 M KCl using the Available Nitrogen Extraction SOP from Soil Sample. Results:

[00108] As shown in Table 4, the total nitrogen (N) content of the acidulated samples increases as the urea pretreatment concentration increases from a 0.3:1 ratio to a 0.6:1 urea:biomass ratio and finally to a 1:1 urea:biomass ratio. At all urea concentrations, the washed samples showed N content similar to that of their pre-ammoniated counterparts. This means that the nitrogen from the urea is bound to the carbon matrix of the acidulated pine wood chips, thus retaining N even after washing.

[00109] Table 4 also shows a higher N retention in the ammoniated washed samples at a 0.3:1 urea:biomass ratio and at a 0.6:1 urea:biomass ratio when compared to non-ammoniated washed samples at the same respective concentrations. This increase in N retention after ammoniation and washing was also observed in the arginine pretreatment sample. Without limiting oneself to any particular theory or mechanism of action, the higher N retention of the ammoniated samples after washing can be explained by the ammonium cation (NH4+) of aqueous ammonia that Petition 870250099571, dated 10 / 30 / 2025, page 35 / 69 28 / 54 forms an ionic bond with the negative sites of the acidulated carbon. The nitrogen difference between the pretreatments with a urea:biomass ratio of 0.3:1 and urea:biomass of 0.6:1 is 30% and 36%, respectively, of the original nitrogen content before washing.

[00110] Table 4 shows that the arginine pretreatments showed lower total N content. Unlike the pretreatments with increased urea concentration, the arginine pretreatments showed only a slight increase in total N with increasing arginine concentration. This can be explained by the lower N content in arginine versus urea and other pretreatments.

[00111] Table 4 shows that the lysine and polyacrylamide pretreatments have low N content after acidification and had little or no N content after washing, suggesting that there was no N binding to the carbon matrix.

[00112] The results shown in Table 4 suggest that the chemical structure of the pretreatment source contains an activated carbonyl group, for example, in urea, or an imine group, for example, in arginine. This is not a theory, but during carbonization, oxygen portions on the carbon surface are created as alcohols or carboxylic acids that react chemically with the pretreatment chemical to form carbamate-like bonds on the carbon surface, binding to the nitrogen source. Other pretreatments, such as ammonia or lysine, do not possess these activated carbonyl or imine groups and exhibit little or no nitrogen retention in the washed samples. Table 4: Results of combustion analysis of acidified, ammoniated and washed pine wood chips, pre-treated with urea, arginine, lysine, aqueous ammonia or polyacrylamide at various concentrations. (*) indicates that the sample exceeded the calibration range. Petition 870250099571, dated 10 / 30 / 2025, p. 36 / 69 29 / 54 Pretreatment Treatment with Pretreated Biomass Combustion Analysis (%) TC TN TS 0.3:1 urea:acidified biomass 33 6.1 13* 0.3:1 urea:acidified biomass, after washing 47 6.7 3.8 3.1: urea: acidified biomass Ammonized 33 38 8.7 0.3:1 urea:biomass Acidulated and ammoniated, then washed 56 10 4.0 0.6:1 urea:acidified biomass 37 9.7 16* 0.6:1 urea:acidified biomass, then washed 0.6:1 of urea:acidified and ammonized biomass 38 42 6.5 0.6:1 of urea:acidified and ammonized biomass, after washing 43 12 5.7 1:1 of urea:acidified biomass 21 12 15* urea: 1:1 of acidified biomass, after washing 48 11 6 0.3:1 of arginine:acidified biomass 33 4.4 10* 0.3:1 of arginine:acidified biomass, after washing 43 6, 8 5.6 0.3:1 of arginine:acidified and ammonized biomass 35.7:35 arginine:acidified and ammonized biomass, then washed 48 12 6.0 0.6:1 of arginine:acidified biomass 18 5.5 16 0.6:1 of arginine:acidified and ammonized biomass 23 32 8.4* 0,6:1 of arginine:biomass Acidulated and ammoniated, then washed 40 10 4.7 0.3:1 of lysine:biomass Acidulated 39 3.2 11* 0.3:1 of lysine:biomass Acidulated, then washed 47 0.96 5.4 0.3:6 of lysine:biomass acidulated 3.3 11* 0.6:1 lysine:biomass Acidulated, then washed 50 1.1 5.5, Petition 870250099571, of 30 / 10 / 2025, p. 37 / 69 30 / 54 1:1 lysine:acidified biomass 24 4.8 11* 1:1 lysine:acidified biomass, then washed 41 0.93 4.7 0.3:1 polyacrylamide:acidified biomass 29 0.74 12* 0.3:1 polyacrylamide: acidified biomass, then washed 52 3.2 5.0

[00113] Table 5 shows that the duration of immersion time for the 0.6:1 urea:biomass and 1:1 urea:biomass pretreatment solutions had a minimal effect on the N content after acidification. The acidified samples of 0.6:1 urea:biomass at all immersion times: 1 day, 3 days, 1 week and 4 weeks, initially had an N content around the 8-10% range, but after washing, it was shown that 1-day immersion and 3-day immersion have a higher N content than immersion for more than 1 week. Table 5: Results of the combustion analysis of acidulated and washed pine wood chips pre-treated with 0.6:1 urea:biomass or 1:1 urea:biomass solutions with various pre-treatment immersion times. (*) indicates that the sample exceeded the calibration range. Sample Combustion Analysis (%) TC TN TS 0.6:1 urea:biomass - 1 day immersion 20 8.5 16* 0.6:1 urea:biomass - 1 day immersion - washed 47 8.5 3.1 0.6:1 urea:biomass - 3 days immersion 37 9.7 16* 0.6:1 urea:biomass - 3 days immersion - washed 45 9.1 5.3 0.6:1 urea:biomass - 1 week immersion 40 10 12* 0.6:1 urea:biomass - 1 week immersion - washed 68 6.7 6.3 Petition 870250099571, dated 10 / 30 / 2025, pp. 38 / 69 31 / 54 0.6:1 urea:biomass - 4 Weeks Immersion 47 9.3 14* 0.6:1 urea:biomass - 4 Weeks Immersion - Washed 18 6.3 3.5 1:1 urea:biomass - 1 day immersion ^^^B ^^^B ^^^B 1:1 urea:biomass - 1 day immersion - washed 45 12 8.3* 1:1 urea:biomass - 3 days immersion 21 12 15* 1:1 urea:biomass - 3 days immersion - washed 48 11 6.0

[00114] Table 6 shows the total N content of the CCT pretreated with a 0.6:1 urea:biomass solution when washed with DI water or 2 M KCl. The sample washed with 2 M KCl showed a higher N content than the sample washed with DI water and the acidified washed sample. This suggests that N and S are strongly (i.e., covalently) bound in the carbon matrix, as any ionically bound nitrogen would be removed by washing with KCl. Table 6: Results of the combustion analysis of CCT pretreated with 0.6:1 urea:biomass, washed with DI water and 2 M KCl. Sample Combustion Analysis (%) TC TN TS 0.6:1 urea:biomass, Acidulated - Washed 45 9.1 5.3 0.6:1 urea:biomass, acidified and then ammoniated - washed with water DI 43 12 5.7 0.6:1 urea:biomass, acidified and then ammoniated washed with 2 M KCl 35 15 7.5

[00115] The results of the ion chromatography of the filtrate extracted from the CCT sample pre-treated with 0.6:1 urea:biomass are shown in Table 7. Increasing the concentration of the extracting solution did not appear to increase the amount of ammonium ion extracted, indicating that nitrogen Petition 870250099571, dated 10 / 30 / 2025, pp. 39 / 69 32 / 54 is strongly linked to the carbon complex. Table 7: Results of ion chromatography (IC) extraction of CCT with pretreatment with 0.6:1 urea:biomass. The sample was extracted with DI water, 0.5 M KCl and 2 M KCl using the SOP for Available N Extraction in Soil Sample. Washing Procedure | Ion Chromatography Filtrate Results (ppm) | SO42- | SO42- | -S | NH4+ | Washed with Water | DI | 103650.00 | 34515.45 | 2658.20 | Washed with 0.5 M KCl | 103116.30 | 34337.73 | 2809.54 | Washed with 2 M KCl | 89903.55 | 29937.88 | 2730.12

[00116] In summary, urea pretreatment prevails among all other pretreatments in retaining the highest total N content after washing. From the extraction of 2 M KCl from the sample pretreated with 0.6:1 urea:biomass, it is suggested that nitrogen is strongly bound to the porous carbon matrix. EXAMPLE 3: Effect of the Order of Hydrogen Peroxide Addition to Carbonaceous Biomass Pretreatment Methods

[00117] Experiments were conducted to investigate the effect of adding hydrogen peroxide before nitrogen treatment on nutrient retention of the resulting porous carbon matrix product.

[00118] Solutions of varying concentrations of hydrogen peroxide were tested as a pretreatment for carbonaceous biomass samples (e.g., pine wood chips) at concentrations of 15%, 30%, and 50% w / w with the subsequent addition of a urea solution (0.6:1 urea:biomass on a dry weight basis) followed by acidification.

[00119] During acidification, sulfuric acid (1:1 acid:biomass by weight) was slowly added to the chips of Petition 870250099571, dated 10 / 30 / 2025, p. 40 / 69 33 / 54 pine wood. The resulting acidified porous carbon matrix samples were slowly stirred manually with a glass rod for 5 minutes or until all pine wood chips were coated / reacted.

[00120] The nitrogen-treated and acidified porous carbon matrix samples were slowly added to the aqueous ammonia solution and manually stirred with a glass rod for 5 minutes or until all the pine wood chips were coated / reacted to neutralize the residual acid. The highest temperature of the ammoniation reaction was recorded. The samples were then partitioned for combustion analysis. The samples were dried at 70 °C overnight before combustion analysis.

[00121] The samples were then washed using vacuum filtration and monitored by pH and EC to ensure complete washing. The samples were then dried in an oven at 70 °C overnight. The samples were weighed and then partitioned for analysis by combustion analysis. Results:

[00122] As shown in Table 8, the total retained nitrogen (N) content of the acidified samples increased with the addition of 15% hydrogen peroxide, but increased only slightly when the peroxide was increased to 30% and 50%. This suggests that the addition of oxygen functionality to the carbon surface increases N retention. This would further mean that N is being bound to the carbon surface via oxygen moieties, as previously suggested. Table 8: Effect of pretreatment with hydrogen peroxide. Pretreated Biomass Combustion Analysis (%) CNS 0.6:1 urea:biomass, acidified 37 9.7 16* 0.6:1 urea:biomass, acidified - washed 45 9.1 5.3 Petition 870250099571, dated 10 / 30 / 2025, page 41 / 69 34 / 54 0.6:1 urea:biomass, Acidulated and then Ammoniated - Washed 43 12 5.7 0.6:1 urea:biomass with 15% Hydrogen Peroxide, Acidulated 44 20 6.8 0.6:1 urea:biomass with 15% Hydrogen Peroxide, Acidulated - Washed 33 12 11* 0.6:1 urea:biomass with 30% Hydrogen Peroxide, Acidulated 44 21 7.9 0.6:1 urea:biomass with 30% Hydrogen Peroxide, Acidulated - Washed 46 10 8.7* 0.6:1 urea:biomass with 30% Hydrogen Peroxide, Acidulated, then Ammoniated Washed 43 11 9.4* 0.6:1 urea:biomass with 50% hydrogen peroxide, acidified 51 20 8.9* 0.6:1 urea:biomass with 20% hydrogen peroxide, acidified, then ammoniated and washed 39 13 7.7 EXAMPLE 4: Effect of Moisture on Carbonaceous Biomass Pretreatment Methods

[00123] Experiments were conducted to investigate the effect of drying prior to acidification on nutrient retention of the resulting porous carbon matrix product.

[00124] Urea solution was added to biomass samples prior to acidification to achieve a urea:biomass ratio of 0.6:1 and immersed for 1 hour. The pre-treated samples were then acidified directly or dried overnight at 70 °C prior to acidification.

[00125] Sulfuric acid was slowly added to pre-treated pine wood chips in a 1:1 ratio of pre-treated biomass to sulfuric acid. The resulting acidified porous carbon matrix sample was slowly stirred manually with a glass rod for 5 minutes or until all the pine wood chips were coated / reacted. The highest temperature of the acidification reaction was recorded.

[00126] The pre-treated and acidified porous carbon matrix samples were slowly added to Aq. Ammonia at a 1:1 Aq. Ammonia:biomass ratio (by weight) and stirred with a Petition 870250099571, dated 10 / 30 / 2025, p. 42 / 69 35 / 54 glass rod manually for 5 minutes or until all pine wood chips were coated / reacted to neutralize residual acid. The CCT samples were then partitioned for combustion analysis. The samples were dried at 70 °C overnight before combustion analysis.

[00127] To measure retained nitrogen and sulfur content in the sample, available / exchangeable N (including ammonium, nitrate, nitrite and soluble organic N) in the CCT was extracted with DI water using the Soil Sample Available N Extraction SOP. Results:

[00128] As shown in Table 9, drying the pretreated material at 70 °C overnight before acidulation had little effect on the nutrient analysis of the final sample after ammoniation. A small difference in acidulation reactivity was observed, but this did not lead to a significant change in the nutrient analysis of the amount of nitrogen retained. Table 9: Results of combustion and N retention on the effect of moisture content on acidification. (*) indicates analysis by the persulfate method. Sample Combustion Results TN TS TC N bound to C % % of original N 0.6:1 urea:biomass, Dry, Acidulated with Sulfuric Acid (1:1), Ammoniated with Aqueous Ammonia (1:1) 22.8 16.8 12.2 37.7* 0.6:1 urea:biomass, Not Dry, Acidulated with Sulfuric Acid (1:1), Ammoniated with Aqueous Ammonia (1:1) 22.5 15.9 12.1 41.2* EXAMPLE 5: Effect of the Order of Addition of Nitrogen Treatment to Carbonaceous Biomass

[00129] Experiments were conducted to investigate the effect of the order of addition of nitrogen treatment on Petition 870250099571, dated 10 / 30 / 2025, page 43 / 69 36 / 54 nutrient retention of the resulting porous carbon matrix product.

[00130] Urea solution was added to biomass samples (i.e., pine wood chips) before acidification and allowed to soak, or after acidification, to achieve a urea:biomass ratio of 0.6:1. During acidification, sulfuric acid was slowly added to the pine wood chips. The resulting acidified porous carbon matrix sample was slowly stirred with a glass rod manually for 5 minutes or until all the pine wood chips were coated / reacted.

[00131] The nitrogen-treated and acidified porous carbon matrix samples were slowly added to the aqueous ammonia solution and manually stirred with a glass rod for 5 minutes or until all pine wood chips were coated / reacted to neutralize the residual acid. CCT samples were then partitioned for combustion analysis. The samples were dried at 70 °C overnight before combustion analysis.

[00132] To measure retained nitrogen and sulfur content in the sample, available / exchangeable N (including ammonium, nitrate, nitrite and soluble organic N) in the CCT was extracted with DI water using the Soil Sample Available N Extraction SOP. Results:

[00133] As shown in Table 10, the amount of nitrogen retained in the porous carbon matrix sample after ammoniation was similar regardless of whether the urea solution (at a ratio of 0.6:1 urea:biomass by weight) was added before or after acidification. Table 10: Results of combustion analysis of acidified and ammoniated CCT samples with N treatment before or after acidification and the effect of the order of urea addition. (*) indicates analysis by the persulfate method. Petition 870250099571, dated 10 / 30 / 2025, page 44 / 69 37 / 54 Sample Combustion Results TN TS TC N bound to C % % of original N Treated with Urea Solution (0.6:1 urea:biomass) Before Acidulation 22.5 15.9 12.1 41.2* Treated with Urea Solution (0.6:1 urea:biomass) After Acidulation 22.4 16.3 12.4 41.9* EXAMPLE 6: Effect of Temperature on Acidulation and Ammoniation

[00134] Experiments were conducted to investigate the effect of temperature on nitrogen retention in the ammoniated sample.

[00135] Urea solution was added to biomass samples (e.g., pine wood chips) prior to acidification to achieve a urea:biomass ratio of 0.6:1 and left to soak for 1 hour. The biomass temperature was then maintained at room temperature (RT) and allowed to rise during acidification (the reaction temperature was not manipulated) or the reaction temperature was maintained at 40 °C during acidification. During acidification, sulfuric acid was slowly added to the pine wood chips and stirred slowly with a glass rod manually for 5 minutes or until all the pine wood chips were coated / reacted.

[00136] Pre-treated and acidified porous carbon matrix samples were slowly coated with aqueous ammonia solution at RT and allowed to increase in temperature during ammoniation (the reaction temperature was not manipulated) or maintained at 40 °C and manually stirred with a glass rod for 5 minutes or until all the acidified material was coated / reacted to neutralize the residual acid. The samples were then partitioned for combustion analysis. The samples were dried at 70 °C overnight before analysis. Petition 870250099571, dated 10 / 30 / 2025, pp. 45 / 69 38 / 54 combustion.

[00137] To measure retained nitrogen and sulfur content in the sample, available / exchangeable N (including ammonium, nitrate, nitrite and soluble organic N) in the CCT was extracted with DI water using the Soil Sample Available N Extraction SOP. Results:

[00138] As shown in Table 11, it can be observed that a lower temperature when the urea solution is mixed with the acid leads to more retained nitrogen. When acidified and ammoniated at 40 °C, the retained nitrogen is about 60% compared to when both acidification and ammoniation reach the increased reaction temperature. In the other samples, when the ammoniation temperature is kept constant at 40 °C and the acidification temperature can be increased, the retained nitrogen also increases when the temperature is kept lower. Table 11: Results of combustion and N retention on the effect of temperature on acidification and ammoniation. (*) indicates analysis by the persulfate method. Sample Combustion Results TN TS TC N bound to C % % of original N 0.6:1 urea:biomass, Dry, Acidulated with Sulfuric Acid (1:1), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammoniation Reaction Temperature not manipulated 22.8 16.8 12.2 37.7* 0.6:1 urea:biomass, Dry, Acidulated with Sulfuric Acid (1:1), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammoniation Reaction Temperature maintained at 40 °C 23.7 9.8 23.2 60.4* 0.6:1 urea:biomass, Not Dry, Acidulated with Sulfuric Acid (1:0.8), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammonification Reaction Temperature Maintained at 40 °C 21.9 15.9 13.5 50.7* Petition 870250099571, dated 10 / 30 / 2025, pp. 46 / 69 39 / 54 0.6:1 urea:biomass, Non-Dried, Acidified with Sulfuric Acid (1:0.8), Ammoniated with Aqueous Ammonia (1:1), Ammoniation Reaction Temperature Maintained at 40 °C 22.1 15.2 14.9 43.7*

[00139] As shown in Table 12, a similar trend was observed between temperature and nitrogen retention. After acidification, the urea solution showed greater nitrogen retention when urea and acid were added at a lower temperature. Additionally, the ammoniation temperature also appears to significantly affect nitrogen retention. Table 12: Results of combustion and N retention on the effect of temperature on acidification and ammoniation. (*) indicates analysis by the persulfate method. Sample Combustion Results TN TS TC N bound to C % % of original N Biomass Acidulated with Sulfuric Acid (1:1.3) at RT, Then Added Urea Solution (0.6:1 urea:biomass), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammoniation Reaction Temperature Not Manipulated 22.4 14.6 15.4 56.5* Biomass Acidulated with Sulfuric Acid (1:1.3) at RT, Then Added Urea Solution (0.6:1 urea:biomass), Ammoniated with Aq. Ammonia (1:1), Acidulation Reaction Temperature Maintained at 40 °C 22.4 16.3 12.4 41.9* Biomass Acidulated with Sulfuric Acid (1:1.3) at RT, Then Added Urea Solution (0.6:1 urea:biomass), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammoniation Reaction Temperature Maintained at 40 °C 23.1 9.9 22.7 60.2* EXAMPLE 7: Effect of Other Acids on Nitrogen Retention

[00140] Experiments were conducted to investigate the Petition 870250099571, dated 10 / 30 / 2025, pp. 47 / 69 40 / 54 effect of other acids on nitrogen retention of the resulting porous carbon matrix product.

[00141] Urea solution was added to biomass samples (e.g., pine wood chips) prior to acidification to achieve a urea:biomass ratio of 0.6:1 and left to soak for 1 hour. The biomass temperature was then maintained at RT and allowed to increase during acidification (the reaction temperature was not manipulated) or the reaction temperature was maintained at 40 °C during acidification. Acidification was achieved with sulfuric acid (SA) and phosphoric acid (PA), where SA was added first and allowed to react, followed by PA. The resulting acidified porous carbon matrix sample was slowly stirred with a glass rod manually for 5 minutes or until all the material was coated / reacted.

[00142] The pre-treated and acidified porous carbon matrix samples were slowly added to the aqueous ammonia solution and held at 40 °C and stirred manually with a glass rod for 5 minutes or until all the material was coated / reacted to neutralize the residual acid. The samples were then partitioned for combustion analysis. The samples were dried at 70 °C overnight before combustion analysis.

[00143] To measure retained nitrogen and sulfur content in the sample, available / exchangeable N (including ammonium, nitrate, nitrite and soluble organic N) in the CCT was extracted with DI water using the Soil Sample Available N Extraction SOP. Results:

[00144] As shown in Table 13, a mixture of acids can be used to produce a product with retained nitrogen. It is observed in this sample that the reaction temperature does not affect the retained nitrogen, possibly due to the mixture of acids. Table 13: Results of combustion and N retention in the effect Petition 870250099571, dated 10 / 30 / 2025, pp. 48 / 69 41 / 54 of the addition of other mineral acids. (*) indicates analysis by the persulfate method. Sample Combustion Results TN TS TC N bound to C % % of original N 0.6:1 urea:biomass, Non-Dried, Acidulated with SA (1:0.8) and PA (1:0.5), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammoniation Reaction Temperature Maintained at 40 °C 21.1 13.0 8.6 27.8* 0.6:1 urea:biomass, Non-Dried, Acidulated with SA (1:0.8) and PA (1:0.5), Ammoniated with Aq. Ammonia (1:1), Ammoniation Reaction Temperature Only Maintained at 40 °C 21.0 12.0 9.6 28.6* EXAMPLE 8: Effect of Metal Addition on Nitrogen Retention

[00145] Experiments were conducted to investigate the addition of metals as a pretreatment on nutrient retention of the resulting porous carbon matrix product.

[00146] Biomass samples were added to a solution of ferrous sulfate or zinc chloride and left to soak for 1 hour. Acidification was achieved with sulfuric acid, which was slowly added to the pine wood chips. The resulting acidified porous carbon matrix sample was slowly stirred manually with a glass rod for 5 minutes or until all the material was coated / reacted.

[00147] The pre-treated and acidified porous carbon matrix samples were then added to a urea solution (urea:biomass ratio of 0.6:1 by weight), followed by an aqueous ammonia solution and stirred manually with a glass rod for 5 minutes or until all the material was coated / reacted to neutralize the residual acid. The samples were then partitioned for analysis by Petition 870250099571, dated 10 / 30 / 2025, pp. 49 / 69 42 / 54 combustion analysis. Samples were dried at 70 °C overnight before combustion analysis.

[00148] To measure retained nitrogen and sulfur content in the sample, available / exchangeable N (including ammonium, nitrate, nitrite and soluble organic N) in the CCT was extracted with DI water using the Soil Sample Available N Extraction SOP. Results:

[00149] As shown in Table 14, metal pretreatment resulted in nitrogen retention within the carbon matrix. When iron sulfate was used, retention of both urea and ammonia was observed. Ammonia retention is possible through complexation with iron within the carbon matrix. No other metal tested retained ammonia. When zinc chloride was used to pretreat the biomass, retention was observed with the addition of the urea solution, but not with ammonia alone. This suggests that iron sulfate forms more complexes with ammonia than zinc chloride. Table 14: Combustion and N retention results in the effect of adding metals as a pretreatment. (*) indicates analysis by the persulfate method. Combustion Results TN TS TC N bound to C % % of original N 10% Iron Sulfate, Undried, Acidulated with SA (1:0.8), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammoniation Reaction Temperature Unmanipulated 9.9 11.7 5.5 12.9* 10% Iron Sulfate, Undried, Acidulated with SA (1:0.8), Urea Solution Added (0.6:1 urea:biomass), Ammoniated with Aq. Ammonia (1:1), Acidulation and Ammoniation Reaction Temperature Unmanipulated 22.1 16.9 29.8 39.3* 10% Zinc Chloride, Undried, Acidulated with SA (1:0.8), Ammoniated with Aq. Ammonia (1:1), Temperature 9.7 11.2 6.7 0.4* Petition 870250099571, dated 10 / 30 / 2025, pp. 50 / 69 43 / 54 Acidulation and Ammonification Reaction Temperature: Unmanipulated 10% Zinc Chloride, Non-Dried, Acidulated with SA (1:0.8), Urea Solution Added (0.6:1 urea:biomass), Ammonified with Aq. Ammonia (1:1), Unmanipulated Acidulation and Ammonification Reaction Temperature: 19.8 16.1 8.4 43.8* EXAMPLE 9: Effect of Temperature Addition on Nitrogen Retention

[00150] Experiments were conducted to investigate the effect of adding temperature at different durations on the nitrogen retention of the resulting porous carbon matrix product.

[00151] Biomass samples (i.e., pine wood chips) were added to a urea solution (2:1 urea:biomass by weight) before acidification and left to soak, or after acidification. During acidification, sulfuric acid (0.25:1 to 1:1 acid:biomass) was slowly added to the pine wood chips and stirred slowly with a glass rod to ensure all chips were coated. The coated biomass was then allowed to rise in temperature due to the exotherm and cool back to room temperature after the reaction, or it was placed in an oven to maintain the exotherm at various temperatures for various periods of time. Acidulations were maintained at different temperatures, including 150 °C, 250 °C, and without the addition of external heat, for a period of 3 to 24 hours. The chosen temperatures were all equal to or less than 250 °C.

[00152] After cooling, the nitrogen-treated and acidified porous carbon matrix samples were slowly filled with aqueous ammonia solution (1:1 Aq. Ammonia:biomass by weight) and stirred manually with a glass rod for 5 minutes or until all pine wood chips were coated / reacted to neutralize residual acid. Samples Petition 870250099571, dated 10 / 30 / 2025, pp. 51 / 69 44 / 54 CCTs were then partitioned for combustion analysis. The samples were dried at 70 °C overnight before combustion analysis.

[00153] To measure retained nitrogen and sulfur content in the sample, available / exchangeable N (including ammonium, nitrate, nitrite and soluble organic N) in the CCT was extracted with DI water using the Soil Sample Available N Extraction SOP. Results: Table 15 shows a comparison of the nutrient analysis between the CCT products produced by urea treatments before or after acidulation at different temperatures. The addition of urea after acidulation, with acidulation maintained at a temperature of 150 °C, produced the highest TN concentration (30.6%) in the CCT products. However, the highest content of N bound to C (82.2%) was achieved when urea was added before acidulation at 250 °C. The addition of heat to the acidulation reaction also produced a higher carbon concentration in the CCT products, with a greater proportion of carbon in a more stable form. This compares to a larger proportion of labile carbon when no heat was added. Changes in the production process involving the acid:biomass ratio, along with temperature and temperature duration, could be refined to alter the proportion of stable and labile carbon in the CCT products, as well as to ensure biomass carbonization. Table 15: Results of combustion analysis of acidified and ammoniated pine wood chips treated with urea. Samples were prepared using various methodologies, as indicated below. (*) indicates analysis by the persulfate method. Products Production Process Combustion Analysis (%) N bound to C Added Urea Solution Heat Used / Acidulation Temperature (°C) Acid:Biomass Ratio (W / W) Acidulation Duration (Hours) TN TS TC % of original N Petition 870250099571, dated 10 / 30 / 2025, pp. 52 / 69 45 / 54 CCT 153 Before Acidulation Yes / 150 0.25:1 24 24.1 3.3 29.9 68.4 CCT 154 Before Acidulation Yes / 250 0.25:1 3 22 4.1 35.4 82.2 CCT 165 Before Acidulation No / 22 1:1 24 28 7.9 20 18.3 CCT 159 After Acidulation Yes / 150 0.25:1 24 30.6 1.1 30.2 13.6 CCT 510 After Acidulation No / 22 1:1 24 22.4 14.6 15.4 56.5* EXAMPLE 10: Measurement of Ammonia Volatilization Reduction in Nitrogen-Treated CCT Products

[00155] Experiments were conducted to investigate whether CCT samples prepared with urea treatment by various methods affect ammonia volatilization. Soil incubation preparation for ammonia volatilization measurement.

[00156] Sandy loam soil (68% sand, 20% silt, and 12% clay) was collected from the surface (0-10 cm) of farmland at various locations near Lethbridge, AB, Canada. The collected soil exhibited an alkaline pH (between 7.5 and 7.8 at a 1:2 soil water extraction ratio), with organic matter of 1.3 to 1.7% and a cation exchange capacity (CEC) of 21.6 to 28.6 meq / 100 g. After removal of coarse root material, the soil was sieved through a 2 mm sieve. A subsample of the soil was used to determine chemical and physical characteristics. The air-dried soil was hydrated to a moisture content of 30% water-filled pore space (WFPS) and pre-incubated in bulk for 48 hours. After pre-incubation, 100 g of soil (oven-dried equivalent) were placed in 1 L glass jars (Mason Jars) before treatment applications.Fertilizer treatments (CCT samples treated with urea and N) were applied to the soil surface to simulate broadcast application in the field at 22.5 mg N / 100 g of soil. Each treatment was replicated three times. The data presented in the tables and figures represent... Petition 870250099571, dated 10 / 30 / 2025, pp. 53 / 69 46 / 54 is the average of three replications with one standard deviation. Urea granules (46-0-0; Greenfield) and CCT-Nitro products (see Table 15 for nutrient analysis) were ground to a similar size before application. The jars were hermetically sealed with a lid and connected to a closed chamber system described below for ammonia volatilization measurements. Ammonia volatilization measurement:

[00157] Ammonia volatilization was measured in a closed chamber system with a constant airflow, with minor modifications to published methods (Miles, 2008 and Woodward, 2008). In summary, ammonia volatilized from the soil surface was retained in a boric acid solution (0.2 M), and the concentration of ammonia retained in boric acid was determined by IC or EC. Ammonia volatilization techniques were described in Miles, 2008 and Woodward, 2008. The soil and fertilizer treatments in the glass jars were then incubated at 25 °C in a closed chamber with a constant airflow of 0.2 L / min. Two sets of boric acid traps (each containing 35 ml of boric acid in 50 ml tubes) were used to capture any ammonia gas emitted from the soil. The second boric acid trap was included to ensure that no ammonia escaped due to possible saturation of the boric acid in the first trap.Boric acid in the traps was changed daily to avoid saturation, and the ammonia concentration in the collected boric acid was measured. Daily ammonia volatilization was calculated by summing the ammonia retained in two sets of boric acid. Ammonia volatilization was measured during the first 8 days of incubation. Results:

[00158] Table 16 shows the cumulative ammonia (NH3) volatilization loss from urea and CCT products revealed in Table 15 in the first 8 days after soil application. Among the four CCT products with different production methods, Petition 870250099571, dated 10 / 30 / 2025, pp. 54 / 69 47 / 54 CCT 153 and 154 showed the greatest reductions in ammonia volatilization; 61% to 82% compared to urea. These products had urea added before acidification at temperatures of 150 °C and 250 °C, respectively, with an acid-to-biomass ratio of 0.25:1. No reductions in ammonia volatilization were observed when no heat was added (CCT 165) and the acid-to-biomass ratio was 1:1. An acidification period of more than 3 hours had little effect on volatilization. Soil with low CEC showed higher volatilization compared to soil with high CEC for urea, but not for CCT 153.

[00159] Urea was dissolved in the soil solution after being applied to the soil and then hydrolyzed into carbon dioxide and ammonium ions by urease enzymes present in the soil. Ammonia volatilization occurs when ammonium ions convert to ammonia in the soil solution due to alkalinity (pH > 7) and the high concentration of ammonium in the soil solution. The ammonia then diffuses out of the soil and is lost to the air and collected in boric acid traps. Losses of up to 33% were found in alkaline sandy loam soil (shown in Table 16), but may be higher or lower in other soil types.Without limiting oneself to any specific theory or mechanism of action, it appears that in the CCT products where urea was added prior to acidification with the addition of heat, the urea bound to the porous carbon matrix more firmly, or in a form inaccessible to the urease enzyme, resulting in less N released into the soil solution, thus reducing ammonium in the soil and subsequent loss as volatilized ammonia. Preventing urease degradation of N bound to the carbon matrix resulted in a substantial decrease in ammonia volatilization from CCT 153 and 154.

[00160] Cumulative ammonia volatilization in Table 16 and Figures 4-6 shows that the introduction of urea before acidification and the addition of heat during acidification reduced ammonia volatilization. Increasing the temperature from 150 °C to Petition 870250099571, dated 10 / 30 / 2025, pp. 55 / 69 48 / 54 250 °C during acidification had little impact and suggests that adding heat or maintaining the exotherm of the acidulation reaction for a period of time with urea added before acidification binds nitrogen more strongly to the porous carbon matrix. Table 16: Cumulative loss of ammonia volatilization from urea and CCT products. ND indicates not determined. Products Production Process Cumulative NH3 Volatilization (% of total N applied) Added Urea Solution Heat Used / Temperature (°C) Acid:Biomass Ratio (W / W) In Soil with a Lower CEC (21.6 meq / 100 g) In Soil with a Higher CEC (28.6 meq / 100 g) Urea N / AN / A / N / AN / A 32.9 20.46 CCT 153 Before Acidulation Yes / 150 0.25:1 6.9 7.9 CCT 154 Before Acidulation Yes / 250 0.25:1 5.9 ND CCT 165 Before Acidulation No / 22 1:1 ND 25.2 CCT 159 After Acidulation Yes / 150 0.25:1 31.3 ND EXAMPLE 11: Evaluation of slow release of N from CCT products

[00161] Experiments were conducted to investigate various slow-release nitrogen CCT products. Soil incubation preparation for evaluation of slow-release nitrogen:

[00162] The slow release of N in N-treated CCT products was evaluated in a laboratory incubation experiment. The experiment used a sandy loam soil, as described in Example 10, and CCT products, as described in Example 9. For the incubation experiment, partially air-dried soil was hydrated to 40% WFPS moisture and pre-incubated at 25 °C for 48 hours to initiate and stabilize microbial activities in Petition 870250099571, dated 10 / 30 / 2025, pp. 56 / 69 49 / 54 soil. After pre-incubation, 50 g of soil (oven-dry equivalent) were placed in 250 mL Nalgene flasks. Fertilizers, including ammonium sulfate (AMS), urea, environmentally smart nitrogen (ESN), and CCT products (see Table 15), were added at a rate of 12.6 mg N / 100 g of soil and thoroughly mixed into the soil with a spatula. No fertilizer was added in a control treatment without N. Each treatment was replicated three times. Deionized water (DI) was added to increase the moisture content to 50% WFPS. The flasks were sealed with perforated aluminum foil to allow air exchange with minimal soil water loss. The soil was then incubated in an incubator at 25 °C in the dark for 56 days. The moisture content was maintained at 50% WFPS throughout the incubation by adding MilliQ water twice a week. The soil was destructively sampled on day 1 (after 24 hours), 7, 14, 28, and 56 of incubation.Separate bottles were prepared for each sampling time. At each sampling time, 3 bottles (each representing a replication) from each treatment were randomly selected, and the soil was then extracted with DI water at a ratio of 1:3 (soil:water, w / w). To ensure accurate sample representation, all the soil (50 g) in the bottle was extracted with 150 ml of DI water, agitating the solution at 150 rpm on a horizontal shaker for 30 minutes. The solution was then filtered through a 45 μm filter, and the filtrate was analyzed by IC for extractable ammoniacal (NH4+), nitrite (NO2-), and nitrate (NO3-) N. Nitrite was below the detection limits in all analyses. Mineral NO released from the fertilizer was calculated by summing ammoniacal-N and nitrate-N in the extract, while the % N recovery was calculated as: The percentage of N recovery was calculated as: Total mineral N(trt)-Total mineral N (control) Total mineral N in treatment (%) =--------------------------------------- x 100 Total N applied to the soil in the treatment Petition 870250099571, dated 10 / 30 / 2025, pp. 57 / 69 50 / 54 The percentage recovery of S was calculated as: SO4---Strt(%) = (S04-S (trt-) - S04-S (control)) Total S applied to the soil Results:

[00163] The nutrient contents of previous CTT samples without treatment with a nitrogen source were in the range of 11-18% N and 11-15% S. With treatment with a nitrogen source, the N content increased regardless of whether urea was added before or after acidification, including by up to 30.6% (CCT 159) (Table 15). Adding more nitrogen before or after acidification is possible to further increase the nitrogen content.

[00164] Table 17 and Figure 7 show that the N released from CCT products after application to the soil depends on the production method, indicating that the nitrogen retained by the porous carbon matrix is ​​in different forms depending on the production method. For example, carbon can occur in a labile or stable form. When heat is added during acidification, more stable carbon is produced, and when urea is added before acidification, the N reacts with this stable carbon during carbonization. When this product is applied to the soil, the reacted N is released more slowly than the N that is soluble or the N that is bound to labile carbon. In our tests, the three CCT products treated with N exhibited quite distinct patterns of N release over time in the soil.CCT 165, which was produced by adding urea solution before acidification but without the addition of heat, released N in a pattern similar to AMS and urea, presumably because the N reacted and bound to labile carbon. A similar pattern was shown with CCT 510, which was produced by adding urea solution after acidification. Acidulation of biomass without the use of external heat produced readily soluble N in the CCT products with a high proportion of labile carbon that was released similarly to AMS and urea. Petition 870250099571, dated 10 / 30 / 2025, pp. 58 / 69 51 / 54 urea. When heat was added during acidulation (CCT 154), a much smaller proportion of N was released (only 25.5% of the total N applied) in 56 days of incubation, indicating that N was strongly retained due to the stable portion of the porous carbon matrix. The nitrogen released from this CCT product may be too slow to meet the N uptake requirements of many crops, although it is indicative of the ability to manipulate N release rates for various crop scenarios requiring longer N release times.

[00165] With a lower temperature of 150 °C during the acidulation process, CCT 153 demonstrated the characteristics of an agronomically effective source of slow-release N, relevant to many horticultural and large-scale green space crops. Nitrogen release was 10.5, 30.9, 36.4, 59.9, and 74.5% of the total N applied at 24 hours, 7 days, 14 days, 28 days, and 56 days after application, respectively. CCT 153 contains more than 15% slow-release N compared to AMS and urea (meeting the AAPFCO, 2011 definition for a slow-release product). The results also suggest that the N released by CCT 153 is likely effective in meeting the N demand of various crops while minimizing the risk of environmental losses.For example, modern corn hybrids absorb approximately 60-65% of total N requirements at the VT stage (65-75 days after sowing), 80-85% at the R3 stage (90-95 days after sowing), and 100% at the R5-R6 stage (115-120 days after sowing) (Figure 8). Although N requirements and % N absorption vary according to crops at different growth stages, CCT 153 clearly shows the potential to synchronize N release with crop demand. In this study, ESN was included for reference as a commercially available slow-release product, and CCT 153 demonstrates that it prolongs the slow-release characteristics relative to ESN, with data suggesting changes in yield involving... Petition 870250099571, dated 10 / 30 / 2025, pp. 59 / 69 52 / 54 The acid:biomass ratio, along with temperature and temperature duration, can be refined to tailor specific N release patterns to the intended crop and geography to optimize the synchronization of N release with crop demand. In ESN, N release depends on temperature and coating thickness, but in CCT products, without being limited to any specific theory or mechanism of action, it appears that the mode of action for N release is based on solubility and microbial activity. Furthermore, as the crop grows, the roots release exudates that enhance microbial activity, which may cause faster N release from the carbon matrix of CCT products.

[00166] The slow-release N characteristic of CCT is expected to have a major impact on reducing N losses through 1) nitrate leaching; 2) ammonia gas loss; 3) gaseous nitrogen (N2) loss through denitrification; and 4) gaseous nitrous oxide loss – a potent greenhouse gas. Reducing these losses should, in turn, result in increased nitrogen use efficiency and crop yields, while simultaneously reducing the negative environmental impacts of N application in agriculture.

[00167] The data in Table 17 and Figure 7 indicate that CCT production methods should include the addition of urea before acidulation and the addition of heat (150 °C) to produce products with valuable slow-release potential, as demonstrated in CCT 153. Urea added after acidulation during CCT production did not show any slow-release potential, as demonstrated by CCT 510, although the addition of urea after acidulation with heat resulted in a product with a higher N content. The addition of urea before acidulation without CCT with additional heat did not exhibit slow-release characteristics, as shown in CCT 165. Although increasing the temperature during acidulation from the Petition 870250099571, dated 10 / 30 / 2025, pp. 60 / 69 53 / 54 ambient conditions appear to be essential for retaining N in the carbon matrix, a temperature of 250 °C resulted in slower N release than ideal for effective agronomic performance.

[00168] Without being limited to any specific theory or mechanism of action, for CCT products pretreated with urea solution before acidulation, the addition of heat to the acidulation reaction binds N to the porous carbon matrix to produce a slow-release product. Table 17: Cumulative N released (% of total N applied) during 56 days of incubation in the soil. Products Production Process Cumulative N Released on Day 56 (% of Total N Applied) Urea Solution Added Heat Used / Acidulation Temperature (°C) Acid:Biomass Ratio (W / W) Acidulation Duration (Hours) AMS NA N / A / N / A NA NA 104 (5.0) Urea NA N / A / N / A NA NA 92.2 (3.5) ESN NA N / A / N / A NA NA 110.6 (3.5) CCT 153 Before acidification Yes / 150 0.25:1 24 74.6 (3.4) CCT 154 Before acidification Yes / 250 0.25:1 3 25.5 (1.3) CCT 165 Before acidification No / 22 1:1 24 98.4 (6.0) CCT 510 After acidification No / 22 1:1 24 92.5 (1.6)

[00169] Although the disclosure has been described with reference to certain specific embodiments, various modifications thereof will be apparent to those ordinarily versed in the art. All examples provided herein are included solely for the purpose of illustrating the disclosure and are not intended to limit the disclosure in any way. All drawings provided in this document are solely for the purpose of illustrating various aspects of the disclosure and are not intended to be drawn to scale or to limit the disclosure in any way. The scope of the appended claims shall not be limited by the embodiments Petition 870250099571, dated 10 / 30 / 2025, pp. 61 / 69 54 / 54 preferred interpretations set forth in the description above, but should be given the broadest interpretation consistent with this descriptive report as a whole. The disclosures from all documents cited in this document are incorporated herein by reference as if presented in full. REFERÊNCIAS 1. Bender, R.R., Haegele, J.W., Ruffo, M.L. e Below, F.E., 2013. Modern corn hybrids’ nutrient uptake patterns. Better crops, 97(1), pp.7-10. 2. Brian De Borba, Richard F. Jack, e Jeffrey S. Rohrer, 2016. Determination of Total Nitrogen and Phosphorus in Wastewaters by Alkaline Persulfate Digestion Followed by IC. Thermo Fisher Scientific, Sunnyvale, CA, EUA. 3. Maynard, D.G. e Y.P. Kalra. 1993. Nitrogen and exchangeable ammonium nitrogen. p. 25-26. Em M.R. Carter (ed.) Soil Sampling and Methods of Analysis. Lewis Publ., Boca Raton, FL. 4. Miles, D.M., Owens, P.R., Moore Jr, P.A. e Rowe, D.E., 2008. Instrumentation for evaluating differences in ammonia volatilization from broiler litter and cake. Journal of applied poultry research, 17(3), pp.340-347. 5. Omara, P., Aula, L., Oyebiyi, F., e Raun, W.R. 2019. World cereal nitrogen use efficiency trends: review and current knowledge. Agrosystems, Geosciences & Environment, 2(1), pp.18. 6. Woodward, T.R., Frame, W.H., Alley, M.M., Whitehurst, G.B. e Whitehurst, B.M., 2011. Design and validation of a laboratory system for measurement of volatilized ammonia. Agronomy Journal, 103(1), pp.38-44. Petição 870250099571, de 30 / 10 / 2025, pág. 62 / 69

Claims

1 / 3 CLAIMS 1. A method for producing a porous carbon matrix product from a carbonaceous biomass material, characterized in that it comprises: (a) treating the carbonaceous biomass material with at least one nitrogen-containing compound; (b) applying a mineral acid to the carbonaceous biomass material while mixing both components for a period of time, thereby leaving the mineral acid impregnated in the carbonaceous biomass material and covalently linking the nitrogen-containing compound to the carbonaceous biomass material; and (c) converting the mineral acid into its corresponding salt by exposing the acid-impregnated carbonaceous biomass material to ammonia, wherein the porous carbon matrix product contains nitrogen covalently linked to the porous carbon matrix.

2. Method according to claim 1, characterized in that step (b) is performed before step (a).

3. Method according to claim 1, characterized in that the covalently bonded nitrogen is from the nitrogen-containing compound and / or the salt.

4. Method, according to claim 1, characterized in that the carbonaceous biomass material comprises wood, digested, composted or raw animal manure, lignocellulosic materials, agricultural residues, agricultural by-products, organic residues, organic by-products, peat, bagasse, palm oil residues, palm oil by-products, straw, municipal solid waste, bedding materials containing manure, food residues and by-products, nut shells or coconut fiber.

5. Method according to claim 5, characterized in that the wood comprises wood chips, wood pulp or wood powder.

6. A method according to claim 1, characterized in that at least one nitrogen-containing compound is present in an aqueous solution.

7. Method according to claim 1, characterized in that at least one nitrogen-containing compound comprises: an active or available carbonyl or imine group; and / or urea.

8. A method according to claim 7, characterized in that at least one nitrogen-containing compound comprises urea in an amount to achieve a specified nutrient profile.

9. Method according to claim 1, characterized in that step (b) further comprises the application of heat, in addition to the application of the mineral acid.

10. Method according to claim 1, characterized in that the mineral acid is sulfuric acid, nitric acid, phosphoric acid, polyphosphoric acid, hydrochloric acid and / or a combination thereof.

11. Method according to claim 1, characterized in that the ammonia is ammonia gas or aqueous ammonia.

12. Method according to claim 1, characterized in that step (c) comprises flowing an ammonia gas or aqueous ammonia over or through the acid-impregnated carbonaceous biomass material.

13. Method according to claim 1, characterized in that the salt is ammonium sulfate, ammonium nitrate, ammonium phosphate or ammonium chloride.

14. Method according to claim 1, characterized in that it further comprises: before carrying out steps (a), (b) and (c), grinding the carbonaceous biomass material to a suitable particle size range; and / or after step (c), selecting, pelletizing or granulating the porous carbon matrix product to a suitable particle size range.

15. Porous carbon matrix product, characterized in that it is produced by the method as defined in any one of claims 1 to 14.

16. Slow-release fertilizer product, characterized in that it comprises a porous carbon matrix and at least one nitrogen-containing compound covalently bonded to the porous carbon matrix, wherein the porous carbon matrix is ​​impregnated with an ammonium mineral acid salt.

17. Slow-release fertilizer product according to claim 16, characterized in that at least one nitrogen-containing compound comprises: an active or available carbonyl or imine group; and / or urea.

18. Slow-release fertilizer product according to claim 16, characterized in that the mineral acid is sulfuric acid, nitric acid, phosphoric acid, polyphosphoric acid, hydrochloric acid and / or a combination thereof.

19. Slow-release fertilizer product according to claim 16, characterized in that at least one nitrogen-containing compound is released from the fertilizer due to microbial activity over the course of a growing season.

20. Porous carbon matrix product according to claim 15, or slow-release fertilizer product according to any one of claims 16 to 19, characterized in that the porous carbon matrix product or the slow-release fertilizer product reduces ammonia volatilization. Petition 870250099569, dated 10 / 30 / 2025, p. 11 / 16

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