Production and formulation process of standard vegetable charcoal briquettes for hookah and / or liturgical charcoal

Description

1 / 36 PRODUCTION AND FORMULATION PROCESS OF STANDARD VEGETABLE CHARCOAL BRIQUETTES FOR HOOKAH AND / OR LITURGICAL CHARCOAL FIELD OF THE INVENTION

[001] The present invention describes the production process of a new standard hookah charcoal briquette and liturgical charcoal, as well as a new formulation, which advantageously ensures improved characteristics to the product.

[002] The invention described in this document applies to the tobacco products industry. FUNDAMENTALS OF THE INVENTION

[003] The habit of smoking hookah, also known as shisha or arguile, is an ancient practice that has roots in various cultures around the world. Its history dates back centuries to the Middle East and India, initially used as part of social and religious traditions and later spreading to other parts of the world, including Europe, North America and South America, where it is considered a social activity.

[004] In this context, ensuring a good hookah experience therefore depends on choosing the most suitable elements, with charcoal being of extreme importance.

[005] Additionally, liturgical charcoal, normally used in thuribles during ecumenical celebrations, presents Petition 870250002351, dated 10 / 01 / 2025, page 7 / 56 2 / 36 several common characteristics in relation to the charcoal used for hookah. This is because it also needs to light quickly and have high calorific value, and should remain lit throughout the entire celebration.

[006] Furthermore, the charcoal used in liturgies generally remains in contact with other materials, such as herbs, incense or grains, and therefore needs to be heated in order to release their aroma without burning them.

[007] Thus, liturgical charcoal must be more incandescent than ordinary coals, and extinguish itself only after it has been completely consumed.

[008] Currently, the main producers of hookah charcoal and liturgical charcoal are concentrated in Southeast Asia, and countries such as Indonesia, Vietnam, and the Philippines are the main producers. In these countries, this type of charcoal is generally produced from coconut charcoal due to its clean combustion and neutral aroma.

[009] Charcoal production, in general, can have variable ingredients depending on the type of intended use. Thus, for the production of charcoal commonly used in hookah, the basic ingredients are: (1) Coconut shells and (2) Binding substances, responsible for binding the coconut shells together during the manufacturing process. Similarly, in liturgical charcoals, bamboo is commonly used as biomass. Petition 870250002351, dated 10 / 01 / 2025, page 8 / 56 3 / 36

[0010] Although the ingredients used in the manufacture of hookah charcoal and liturgical charcoal are already known, the combination of these ingredients in order to obtain increasingly suitable formulas, such as those that have better burning potential, generate less ash and volatilize fewer toxic substances, is not only desirable, but also a differentiating factor in this market.

[0011] Aiming to obtain a product that guarantees desirable burning qualities and a good user experience, the present invention comprises a process for producing a single charcoal suitable for burning in hookahs and also liturgical settings, as well as a formulation for such charcoal. It is relevant to point out that obtaining a charcoal formulation that performs better than those already described in the prior art is neither obvious nor trivial, requiring experimentation and technical analysis.

[0012] Thus, the present invention describes an optimized formula for the production of charcoal briquettes with potential use in hookah or liturgical settings, which allows obtaining a product with similar or greater effectiveness than the products used as a reference in the prior art.

[0013] Additionally, the present invention also describes a possible formulation that allows obtaining charcoal that, surprisingly, does not require resin containing phenol formaldehyde, substances that, Petition 870250002351, dated 10 / 01 / 2025, p. 9 / 56 4 / 36 Although it is a binding agent, it can also have a toxic effect and is often present in charcoal formulations, especially those used in hookahs.

[0014] Regarding the state of the art, invention PI1001123-4 describes an additive-enhanced charcoal composition and corresponding manufacturing process, which uses potassium nitrate, ferric oxide, metallic silicon, carboxymethylcellulose, ethylcellulose, and graphite powder to increase its temperature and burning time and improve its initiation. The present invention, in turn, uses a reduced quantity of ingredients, in relation to this technology, guarantees high calorific value and a burning time that can reach more than 170 minutes.

[0015] Invention BR 102021005872-2, in turn, describes processes for producing biochar, bio-oil and briquettes from the residual biomass of baru and jatobá fruits, products obtained and uses. The present invention, in turn, comprises the use of babassu coconut husk which, combined with the binders described in this document, guarantees a longer burning time.

[0016] Additionally, it should be noted that, due to the limited technical literature regarding the performance of charcoal briquettes for hookah or even liturgical charcoal, an experimental analysis was carried out with briquettes from a leading market brand, in order to compare the yield of the product described in Petition 870250002351, dated 10 / 01 / 2025, p. 10 / 56 5 / 36 present invention and seek performance superior to that presented by such product. BRIEF DESCRIPTION OF THE INVENTION

[0017] The present invention describes the production process of a new charcoal briquette suitable for use in hookah or liturgical applications, as well as a new formulation which advantageously ensures improved characteristics to the product.

[0018] According to the process described in the present invention, the biomass used for the production of the charcoal briquette is babassu coconut residue, preferably babassu coconut, but not necessarily limited to it.

[0019] The charcoal briquette presented in this document has optimized characteristics that allow its use in hookah, as well as liturgical charcoal. Thus, the choice of substances included in the formulation, as well as the proportion of these ingredients, seek to provide the best experience to the user when using the product.

[0020] According to the present invention, two formulations are presented, the first being characterized by comprising fine babassu coconut charcoal of different grammages combined with 3 different binding substances, such as: Cassava Starch (FM), Resin containing Phenol Formaldehyde (FF) with low Petition 870250002351, dated 10 / 01 / 2025, page 11 / 56 6 / 36 Free formaldehyde emission and White Clay (BC). In addition, the formulation also includes the addition of Titanium Dioxide (TD), a substance that is inert to the ingredients of the composition, as well as to the mechanical resistance and calorific value of the charcoal briquette, but which, however, allows the bleaching of the ashes generated during combustion.

[0021] The production process for optimized charcoal briquettes suitable for use in hookahs, as well as liturgical charcoal, involves the production of briquettes with an average total mass of 50g.

[0022] According to the present process, the material to be briquetted, fine charcoal from babassu coconut waste, binders and titanium dioxide, in the established proportions, are mixed, inserted into the briquetting machine and pressed between 350 and 450 bar, preferably 403 bar in the briquette (40 bar on the manometer), for between 1 and 20 minutes, preferably 15 minutes, and the pressing temperature varies between 50°C and 100°C, preferably between 70°C and 80°C. After the pressing period, the charcoal briquette is kept in an oven for between 1 hour and 48 hours, preferably for 24 hours, and the temperature varies between 70°C and 120°C, preferably 105°C.

[0023] After this process, the briquette is packaged and sent for sale. Petition 870250002351, dated 10 / 01 / 2025, page 12 / 56 7 / 36 BRIEF DESCRIPTION OF THE FIGURES

[0024] Figure 1 shows the process of incorporating the binder into the coal fines, following predetermined formulations, from 1 to 17, as described in Table 1. In Figure 1(A), the mixing carried out manually with a glass rod for 15 minutes can be observed, and in Figure 1(B) it is possible to observe the insertion of the ready-made formulations, one by one, into the cylindrical compartment of the briquetting machine, for the formation of the briquette.

[0025] Figure 2(A), in turn, shows the laboratory briquetting machine with a cylindrical mold, in a hydraulic press that was used to make the briquettes. Figure 2(B) shows the cylindrical mold and press.

[0026] Figure 3(A) shows an example of the briquettes produced for experimental analysis of the present invention and, in Figure 3(B), a briquette from Reference 2 is shown, used for comparison of technical parameters.

[0027] Figure 4 shows the leveling of the briquettes by means of longitudinal sanding so that the upper and lower parts were in direct contact with the equipment, as can be seen in Figure 4(A) and then, in Figure 4(B), the measurement of the length and diameter of the briquettes can be seen, using a digital caliper, to calculate the area of ​​the test specimen. Petition 870250002351, dated 10 / 01 / 2025, page 13 / 56 8 / 36

[0028] Figure 5 shows the test specimen placed in the universal testing machine in the longitudinal position.

[0029] In turn, Figure 6 shows some briquettes that were tested until the specimen collapsed, detected by the rupture of the piece. DETAILED DESCRIPTION OF THE INVENTION

[0030] The present invention describes the production process of a new charcoal briquette suitable for use in hookah, both as liturgical charcoal, as well as a new formulation that advantageously guarantees improved characteristics to the product compared to the state of the art.

[0031] It is important to point out, however, that due to the limited technical literature regarding the performance of charcoal briquettes for hookah or liturgical charcoal, an experimental analysis was carried out with briquettes from a leading market brand, in order to compare the performance of the product described in the present invention and to seek performance superior to that presented by such product.

[0032] In this case, two reference brands in the Brazilian market were used, one of which is produced in the country (presented in this document as Reference 1) and another, in which the material is produced abroad and imported to be sold in the national market (presented in this document as Reference 2). Petition 870250002351, dated 10 / 01 / 2025, page 14 / 56 9 / 36

[0033] Neither of the two products (Reference 1 or Reference 2) publicly describes its composition, so it was not possible to compare these formulas with the one described in this document.

[0034] Among the characteristics presented by the present invention, it is relevant to highlight that the burning time and power proved to be superior to the references analyzed.

[0035] According to the process described in the present invention, the biomass used for the production of the charcoal briquette is coconut residue, preferably babassu coconut residue composed of the epicarp, mesocarp and endocarp, excluding the kernels, but not necessarily limited to them.

[0036] The charcoal briquette presented in this document has optimized characteristics for use in hookahs, as well as for liturgical charcoal. Therefore, the choice of substances included in the formulation, as well as the combined proportion of these ingredients, seeks to provide the best experience for the user when using the product.

[0037] Thus, the present invention describes two formulations, the first being characterized by comprising fines of babassu coconut residue charcoal of different particle sizes combined with 3 different binding substances in established relative proportions, such as Petition 870250002351, dated 10 / 01 / 2025, page 15 / 56 10 / 36 as: Cassava Starch (CM), Phenol Formaldehyde-containing Resin (PF) with low free formaldehyde emission and White Clay (WC). In addition, the formulation also includes the addition of Titanium Dioxide (TD), a substance inert to the ingredients of the composition, as well as to the resistance and calorific value of the charcoal briquette, but which, however, allows the bleaching of the ashes generated during combustion.

[0038] According to the present invention, the formulation of charcoal briquettes suitable for use in hookah and also as liturgical charcoal comprises that the charcoal fines from coconut residues, preferably babassu coconut, are homogeneously surrounded by binders in the variable proportion of (1) 5 to 12% cassava starch; (2) between 0 and 7% phenol formaldehyde-containing resin with low free formaldehyde emission; (3) between 2 and 3.5% white clay, plus (4) up to 1% titanium dioxide.

[0039] Preferably, the present invention comprises that the fine charcoal from babassu coconut waste is homogeneously surrounded by binders in the variable proportion of (1) 5 to 6% cassava starch; (2) 5 to 6% resin containing phenol formaldehyde with low emission of free formalin; (3) 1 to 3% white clay, in addition to (4) up to 1% titanium dioxide.

[0040] Additionally, the formulation described in the present invention may also comprise coal fines. Petition 870250002351, dated 10 / 01 / 2025, page 16 / 56 11 / 36 vegetable waste from babassu coconut is homogeneously surrounded by binders in varying proportions of (1) between 9 and 11% cassava starch; (2) 0% resin containing phenol formaldehyde with low emission of free formaldehyde; (3) between 1 and 3.5% white clay, in addition to (4) between 0.1 and 0.5% titanium dioxide, in relation to the total mass of the briquette.

[0041] The production process for optimized charcoal briquettes suitable for use in hookahs or as liturgical charcoal involves the production of briquettes with an average total mass of 50g.

[0042] According to the present process, the material to be briquetted, fine charcoal from babassu coconut residue, binders and titanium dioxide, in the established proportions, are mixed, inserted into the briquetting machine and pressed between 350 bar and 450 bar in the briquette, preferably 403 bar in the briquette (40 bar on the manometer) for between 1 and 20 minutes, preferably 15 minutes, and the pressing temperature varies between 50°C and 100°C, preferably between 70°C and 80°C. After the pressing period, the charcoal briquette is kept in an oven for between 1 hour and 48 hours, preferably for 24 hours, and the temperature varies between 70°C and 120°C, preferably 105°C.

[0043] After this process, the briquette is packaged and sent for sale. Petition 870250002351, dated 10 / 01 / 2025, p. 17 / 56 12 / 36

[0044] It is worth noting that the final product obtained, according to the formulation proposed in the present invention, guarantees a burning time at average temperature and a total time that are superior to those found in similar products available to the consumer.

[0045] More specifically, the present invention allows the charcoal briquette to remain lit for more than 150 uninterrupted minutes and at a temperature above 550°C throughout the burning period.

[0046] It is also worth noting that, during the burning period, the charcoal briquette, when used in censers for ecumenical celebrations, promotes the release of the aroma of herbs, incense and grains throughout the celebration period, without causing them to burn. EXAMPLES Example 1 - First formulation of ingredients for the production of charcoal briquettes.

[0047] Figure 1 illustrates the process of incorporating the binder into the coal fines, following predetermined formulations, from 1 to 17, as described in Table 1. Table 1: Experimental design for briquettes bonded with three binders together. Formulation: Cassava Starch (%FM) Phenol Formaldehyde (%FF2O2) White Clay (%AB) 1 3 4 2 2 9 4 2 Petition 870250002351, dated 10 / 01 / 2025, page 18 / 56 13 / 36 3 3 10 2 4 9 10 2 5 3 4 5 6 9 4 5 7 3 10 5 8 9 10 5 9 0 7 3.5 10 12 7 3.5 11 6 1 3.5 12 6 13 3.5 13 6 7 0.5 14 6 7 6.5 15 6 7 3.5 16 6 7 3.5 17 6 ​​7 3.5

[0048] The mixture was carried out manually with a glass rod for 15 minutes (Figure 1a) and, subsequently, the formulations were ready to be inserted, one by one, into the cylindrical compartment of the briquetting machine, for the formation of the briquette (Figure 1b). A laboratory briquetting machine with a cylindrical mold was used, in a hydraulic press (Figure 2b).

[0049] The operating parameters of the briquetting machine were the pressing temperature (80°C), the hydraulic pressure on the manometer of 40 bar and on the briquette the pressing pressure of 403 bar, with a pressing time of 15 minutes, as described. Example 2 - Mechanical characterization of briquettes

[0050] The mechanical characterization of the briquettes of the different formulations was carried out using the diametral compression tensile test, known as tensile strength. Petition 870250002351, dated 10 / 01 / 2025, page 19 / 56 14 / 36 to diametral compression. In this analysis, the compressive stress is determined, that is, the compressive force required to break the briquette in relation to the area of ​​the test specimen.

[0051] The tests were performed on an Instron brand universal testing machine and a 20KN load cell was used. The diametral compression tensile test was based on the ASTM C496 / C496M-17:2017 standard.

[0052] Initially, the briquettes were leveled by longitudinal sanding so that the top and bottom parts were in direct contact with the equipment (Figure 3a). Then, the length and diameter of the briquettes were measured using a digital caliper to calculate the area of ​​the test specimen (Figure 3b). Both data were entered into the Bluehill system of the universal testing machine and the method created was standardized at a sensitivity of 15%, with a loading speed that can range between 0.70 and 1.40 MPa / min.

[0053] The test specimen was placed in the universal testing machine in the longitudinal position, as illustrated in Figure 5.

[0054] The briquettes were tested until the specimen collapsed, detected by the rupture of the piece (Figure 6). Upon collapse of the specimen, the result was displayed on the equipment screen and saved to a file.

[0055] Table 2 shows the results of the diametral compressive stress of the briquettes produced with the 17 Petition 870250002351, dated 10 / 01 / 2025, page 20 / 56 15 / 36 different formulations of the experimental design and of References 1 and 2. Table 2: Diametral compressive stress analysis (MPa) Formulation Diametral Compressive Stress (MPa) 1 2.10 2 4.57 3 3.95 4 7.52 5 1.86 6 6.66 7 3.33 8 1.77 9 0.36 10 8.91 11 4.90 12 4.57 13 4.26 14 4.55 15 3.45 16 5.43 17 5.54 Reference 1 7.86 Reference 2 7.34

[0056] The results in Table 2 show that most of the treatments evaluated presented diametral compression stress lower than References 1 and 2. Only the briquettes from treatments 04 and 10 presented an average diametral compression stress similar to or greater than the references. Example 3 - Characterization of the energy properties of briquettes (immediate analysis):

[0057] These analyses were based on HOLMAN (1994) and the ABNT (Brazilian Association of Technical Standards) standards. Petition 870250002351, dated 10 / 01 / 2025, page 21 / 56 16 / 36 Techniques) and ASTM (American Society for Testing and Materials).

[0058] Each of the formulations was tested in triplicate in a random manner, starting with the determination of moisture, followed by the determination of volatile materials and ash, and finally, the fixed carbon content was determined indirectly.

[0059] For this analysis, initially, the porcelain crucibles were pre-calcined in a muffle furnace and, subsequently, the crucibles were placed in a muffle furnace at 575°C for 4 hours. Then, all the crucibles were placed in a desiccator to reach room temperature and, finally, they were weighed. A) MOISTURE CONTENT (U):

[0060] The moisture content was determined based on ABNT NBR8293:1983 - Mineral coal - Determination of moisture and ASTM D3173-87 - Standard Test Method for Moisture in the Analysis Sample of Coal and Coke.

[0061] Approximately 1.0 g of charcoal fines biomass was weighed into each crucible. It was then placed in a circulating air oven at 105±5°C for 90 minutes. Subsequently, the crucibles were placed in a desiccator and then weighed at room temperature. The moisture content (%U) was calculated according to equation 1: Petition 870250002351, dated 10 / 01 / 2025, p. 22 / 56 17 / 36 %U= zlOo Equation 1

[0062] Where: mi is the mass of the crucible with sample before entering the oven; mi is the mass of the crucible with sample after the oven; mamostra is the initial mass of the sample. B) VOLATILE MATERIAL CONTENT (V):

[0063] The volatile matter content was determined based on ABNT NBR8290 - Mineral coal: Determination of volatile matter content. After the moisture analysis was completed, the same crucibles and samples were used for this analysis.

[0064] The crucibles were placed covered on the door of the muffle furnace, which had been preheated to 950±10°C for 2 minutes to condition them to this temperature, and then placed inside the muffle furnace for 6 minutes.

[0065] Subsequently, the crucibles were placed in the desiccator to cool down, thus allowing the final mass to be determined. The volatile matter content (%V) was calculated using equation 2. %V = x 100 Equation 2 ^sample

[0066] Where: irn: mass of the crucible with sample after moisture removal in the oven; nu: mass of the crucible with Petition 870250002351, dated 10 / 01 / 2025, page 23 / 56 18 / 36 sample after removal of volatile materials; msample: initial mass of the sample. C) ASH CONTENT (Z):

[0067] The ash content was determined based on ABNT NBR8289 - Mineral coal - Determination of ash content.

[0068] After the previous step was completed, the crucibles without lids were placed in a muffle furnace preheated to 575 °C for 4 hours. After this period, the calcined samples were placed in a desiccator until they reached room temperature and constant mass.

[0069] The ash content was obtained using equation 3: %Ashes = (———13 / 100% shows* Equation 3

[0070] Where: % Ash: ash content; mi: ash mass (g); sample: initial mass of the sample (g). D) FIXED CARBON CONTENT (FC):

[0071] The fixed carbon content was determined based on ABNT NBR8299. - Mineral coal: Determination of fixed carbon.

[0072] The determination of fixed carbon is done indirectly, that is, by the difference of 100% minus the sum of the contents of moisture (U), volatile materials (V) and ash (Z). The fixed carbon content (%FC) was then calculated using equation 4. %CF = 100 - (%U + %V + %Z) Equation 4 Petition 870250002351, dated 10 / 01 / 2025, page 24 / 56 19 / 36

[0073] The results should not differ in the determination of the 5% moisture content, the 2% volatile matter content, and the 10% ash content.

[0074] Table 3 shows the results of the immediate analysis of the briquettes produced with the three binders together and of References 1 and 2. Table 3: Results of immediate analyses of the formulated briquettes and references. Formulation Moisture (%) Volatiles (%) Ash (%) Fixed Carbon (%) 1 4.11 15.97 8.78 71.14 2 5.85 19.59 8.27 66.29 3 5.34 16.45 9.66 68.55 4 4.51 20.12 9.04 66.33 5 5.56 15.78 10.98 67.68 6 5.27 20.22 10.89 63.63 7 6.18 17.26 11.12 65.44 8 5.87 17.26 11.15 62.34 9 4.08 20.64 9.80 69.77 10 3.50 16.36 10.19 64.72 11 3.28 21.59 9.45 70.27 12 3.51 17.00 10.62 66.96 13 4.54 18.91 8.25 69.55 14 4.11 17.66 12.96 64.39 15 3.59 18.54 10.38 68.32 16 3.72 17.71 10.49 67.45 17 3.87 18.35 10.42 68.07 Reference 1 2.93 19.29 12.31 65.47 Reference 2 6.94 16.61 1.94 74.51

[0075] As shown in Table 3, only the briquettes from treatments 06, 08, 10, and 14 showed fixed carbon contents lower than the Reference 1 formulation. No treatment showed a fixed carbon content higher than Reference 2. Petition 870250002351, dated 10 / 01 / 2025, page 25 / 56 20 / 36

[0076] Only treatments 02, 04, 06, 09 and 11 showed a higher volatile content than the Reference 1 formulation. Example 4 - Calorific Value Analysis

[0077] To determine the higher heating value (HHV), a Parr brand bomb calorimeter, model 6400, was used. Approximately 1.0 g of the sample and 0.5 g of Nujol type natural oil were weighed directly into the equipment's steel container.

[0078] In turn, for Lower Heating Value (LHV) Analysis, it was calculated using equation 5: PCI = PCS - 9 x (H / 100) x 584.2 Equation 5

[0079] Where: LHV: lower heating value (kcal / kg); HHV: higher heating value (kcal / kg); H: hydrogen content (%) - via elemental analysis.

[0080] Table 4 shows the results of the proximate analysis and higher heating value (HHV) of the briquettes produced with the three binders together and Reference 2. Table 4: Results of the analyses regarding the Higher Heating Value (HHV) and Lower Heating Value (LHV) of the formulated briquettes and References 1 and 2. Formulation PCS (Kcal / kg) PCI (Kcal / kg) 1 6,840.40 6,708.43 2 6,568.67 6,436.70 3 6,741.38 6,609.41 Petition 870250002351, dated 10 / 01 / 2025, page 26 / 56 21 / 36 4 6,631.03 6,499.06 5 6,663.73 6,531.76 6 6,441.16 6,309.19 7 6,518.37 6,386.40 8 6,363.58 6,231.60 9 7,029.08 6,897.10 10 6,520.67 6,388.70 11 6,847.51 6,715.54 12 6,563.55 6,431.58 13 6,767.15 6,635.18 14 6,470.28 6,338.31 15 6,778.62 6,646.65 16 6,744.92 6,612.95 17 6,583.71 6,451.74 Reference 1 6,506.93 6,363.92 Reference 2 7,230.22 7,090.36

[0081] As shown in Table 4, only the briquettes from treatments 01, 09 and 11 showed proximate analysis results and PCS similar to and slightly lower than the briquette from Reference 2. Additionally, only treatments 06, 08 and 14 showed PCS lower than Reference 1. Example 5 - Elemental Analysis

[0082] To determine the elemental composition (%) of carbon (C), hydrogen (H), nitrogen (N), sulfur (S) and oxygen (O) in the samples, an elemental analyzer, Thermo Fisher Scientific, model FLASH SMART CHNS, was used.

[0083] Samples in powder form with a mass of 2-8 mg were analyzed and 2,5-bis(5-tert-butyl-benzoxazol-2-yl)thiophene was used as a standard for the BBOT analysis. Petition 870250002351, dated 10 / 01 / 2025, page 27 / 56 22 / 36

[0084] The equipment programming was done according to the following parameters:

[0085] CHNS: right furnace temperature off, left furnace temperature at 950°C and furnace temperature at 65°C. The analysis cycle time was 720s, the sample injection time was 12s, and the carrier gas was 140mLmin-1 of Helium and 250mLmin-1 of Oxygen, and the reference gas was Helium at 100mLmin-1.

[0086] O: the temperature of the right furnace was 1060°C and the left furnace was off, with the furnace temperature at 65°C. The analysis cycle time was 500s, the sample injection time was 10s, the carrier gas was Helium at 100mLmin-1 and the reference gas was Helium at 100mLmin-1. All gases used were of analytical grade.

[0087] All analyses were performed in duplicate and the solid samples were ground and homogenized in a mortar and pestle.

[0088] Only a few treatments were selected for this analysis, namely: 1, 10 and 15, chosen because they are the minimum (3%), maximum (12%) and central (6%) points, respectively, in relation to the cassava starch binder.

[0089] Briquettes from treatments 12 and 14 were also selected because they represented the maximum point (13%) in relation to the phenol formaldehyde-containing resin binder (FF202) with low free formaldehyde emission and the maximum point (6.5%) in relation to the white clay binder, respectively. Petition 870250002351, dated 10 / 01 / 2025, p. 28 / 56 23 / 36

[0090] Table 5 shows the results of the elemental analyses for each of the briquette formulations evaluated. Table 5: CHONS content of the selected briquettes and References 1 and 2. Formulation C (%) N (%) H (%) S (%) O (%) 1 74.82 0.81 2.42 nd 6.46 10 70.7 0.7 2.68 nd 10.21 12 71.05 1.02 2.59 nd 8.34 14 69.39 0.76 2.54 nd 7.39 15 73.53 0.79 2.32 nd 6.94 Reference 1 70.84 0.83 2.72 nd 13.3 Reference 2 77.68 0.89 2.66 nd 7.32

[0091] Table 5 shows the results of the elemental analysis for CHONS of the selected briquettes and References 1 and 2 and, as can be seen, only treatment 14 showed a carbon content lower than Reference 1. Example 6 - Apparent density of briquettes

[0092] The apparent density - DA of the briquettes was calculated using equation 6: DA = m / V Equation 6

[0093] Where, DA: apparent density of the briquette (g / cm3); m: briquette mass (g); V: briquette volume (cm3).

[0094] An analytical balance was used to determine the mass of the briquettes. In turn, for the Petition 870250002351, dated 10 / 01 / 2025, page 29 / 56 24 / 36 Determining the volume of the briquettes, first, the length and diameter dimensions of the briquettes were measured using a Mitutoyo brand digital caliper, model CD-6 PSX. Then, the volume of the briquettes was calculated using equation 7. The briquettes produced in this project have a cylindrical geometry. V = ((π X r2)) X h) Equation 7

[0095] Where, V: volume of the briquette (cm3); r: radius of the briquette (cm); h: height of the briquette (cm).

[0096] Table 6 shows the results of the apparent density of the briquettes from the 17 treatments and the references. Table 6: Results of the apparent density analysis of the briquettes and the references Formulation DA (g / cm3) 1 1.01 2 0.91 3 0.99 4 1.02 5 0.87 6 1.04 7 0.99 8 1.06 9 0.85 10 0.91 11 0.87 12 0.95 13 0.96 14 0.97 15 0.95 16 0.97 17 0.91 Reference 1 1.04 Reference 2 1.06 Petition 870250002351, dated 10 / 01 / 2025, page 30 / 56 25 / 36

[0097] As can be seen in Table 6, regarding the apparent density of the briquettes, the results were similar for all treatments evaluated, ranging from 0.85 to 1.06 g / cm3. Treatment 9 presented the lowest apparent density (0.85 g / cm3) among the briquette treatments evaluated.

[0098] Only treatments 6 and 8 showed the highest apparent densities and were equal to the apparent density of references 1 and 2, respectively. Example 7 - Briquette combustion performance

[0099] For analysis of the briquette combustion performance, a large aluminum electric stove with a shielded electric resistance, 220 V voltage and 675 W power was used.

[00100] Two metal grates were also used, both to allow the briquettes to burn and to allow the ashes of the lit briquettes to be beaten away. A metal tong was also used, both to handle the lit briquettes from the stove to the grate, and to beat the ashes of the burning briquettes onto the metal grate.

[00101] The briquettes were lit on the electric stove, then turned with the metal tongs to ensure they were fully lit. After being fully lit, the briquettes were transferred to the metal grate. Petition 870250002351, dated 10 / 01 / 2025, p. 31 / 56 26 / 36 using the metal tweezers. At that moment the stopwatch was started.

[00102] To measure the firing temperature of the briquettes, a high-precision digital industrial infrared thermometer with a temperature measurement range of -50 to +800°C was used.

[00103] During this test, the temperature of the briquettes was measured at 15, 30, 45, and 60 minutes of burning. Temperature measurements were taken by positioning an infrared thermometer over the briquettes at a distance of approximately 5 centimeters, where the temperature was measured at two points on each of the 2 briquettes of each formulation tested. Only the maximum temperature measured per briquette treatment was recorded for each of the four time intervals considered. Table 7: Results of the briquette combustion test and reference times. Formulation T (15 min) T (30 min) T (45 min) T (60 min) 1 415 464 Amb Amb 2 490 443 Amb Amb 3 518 599 490 502 4 512 545 516 540 5 480 430 300 Amb 6 526 514 Amb Amb 7 560 580 550 443 8 520 598 525 448 9 490 345 Amb Amb 10 490 560 440 201 11 498 527 Amb Amb 12 565 598 517 508 13 597 601 613 561 14 545 598 600 614 Petition 870250002351, dated 10 / 01 / 2025, p. 32 / 56 27 / 36 15 565 621 614 604 16 652 620 599 603 17 589 616 545 544 Reference 1 578 631 588 602 Reference 2 525 489 590 345

[00104] As described in Table 7, Amb = briquette at room temperature, i.e., extinguished. The analyses were performed in duplicate.

[00105] As can be seen in Table 7, the briquettes from Reference 1 showed higher maximum temperatures than the briquettes from Reference 2, for most measurements, except for the maximum temperature measured after 45 minutes of burning.

[00106] The briquettes from treatments 01, 02, 06, 09 and 11 went out before completing 45 minutes of burning.

[00107] It is relevant to observe the variation obtained in the results that derive from simple variation in the relative proportion of binders for briquette formation. Example 8 - Optimization of briquettes based on performance benchmark

[00108] After the mechanical, energy and combustion performance characterizations of the briquettes relating to the 17 treatments of the experimental design, analysis of variance - ANOVA was performed using Minitab software.

[00109] Eleven mechanical, energy and combustion properties of the briquettes were evaluated as response variables, namely: (Y1) diametral compression stress, (Y2) moisture, Petition 870250002351, dated 10 / 01 / 2025, page 33 / 56 28 / 36 (Y3) volatiles, (Y4) ash, (Y5) fixed carbon, (Y6) higher heating value, (Y7) apparent density, (Y8) temperature at 15 minutes of burning, (Y9) temperature at 30 minutes of burning, (Y10) temperature at 45 minutes of burning and (Y11) temperature at 60 minutes of burning.

[00110] For each of the evaluated response variables, a statistical model was generated using Minitab software, in addition to surface plots and contour plots, for each of the evaluated response variables.

[00111] Based on the statistical models generated, the briquettes were optimized using Minitab software, based on Performance References 1 and 2.

[00112] Thus, these analyses allowed us to obtain 5 more optimized formulations for the production of new briquettes, now called H, I, J, K and L. Additionally, optimized briquettes were also produced without the use of the binder resin containing phenol formaldehyde (PF) - formaldehyde-free, called treatment D.

[00113] The optimized formulations obtained by statistical analysis of the performance data can be seen in Table 8. Table 8: Optimized formulations for charcoal briquettes for hookah. Formulation: Cassava Starch (%FM) Phenol Formaldehyde (%FF2O2) White Clay (%AB) D 10 0 2.5 H 3 6 4.5 I 6.5 6.5 2.5 Petition 870250002351, dated 10 / 01 / 2025, page 34 / 56 29 / 36 J 6.5 10 2.5 K 5 7 2.5 L 5 7 3 Reference 1 7 9 3

[00114] Next, mechanical, energy and combustion performance characterization tests were carried out on these briquettes.

[00115] The validation of these laboratory-scale optimized briquettes was carried out by means of statistical comparison between the means of the evaluated properties of these briquettes, comparing them with the means of the evaluated properties of the briquettes with Reference 1, using Tukey's test, used to test any and all differences between two treatment means.

[00116] Tukey's test was performed only for the variables / properties that were determined in triplicate, i.e., Tukey's test was performed only for moisture, volatiles, ash, fixed carbon and higher heating value (HHV).

[00117] Table 9 shows the diametral compression stress results for the optimized briquettes and References 1 and 2.

[00118] Table 9: Diametral compressive stress of optimized and reference briquettes. Formulation Diametral Compressive Strength (MPa) 5.05 Petition 870250002351, dated 10 / 01 / 2025, p. 35 / 56 30 / 36 H 2.58 I 5.85 J 8.15 K 6.15 L 4.64 Reference 1 7.86 Reference 2 7.34

[00119] The results in Table 9 show that only the average of treatment J was higher than the references. However, for the application of briquettes as hookah charcoal or liturgical charcoal, a diametral compression strength greater than 5 MPa is more than sufficient from a mechanical point of view for this application. Example 9 - Characterization and validation of the energy properties of optimized briquettes A) IMMEDIATE ANALYSIS:

[00120] Table 10 shows the results of the immediate analysis of the optimized briquettes and References 1 and 2.

[00121] According to Table 10, all optimized briquette treatments showed a higher average fixed carbon content than the briquettes from Reference 1, except for treatment D, which was produced without the addition of the phenol-formaldehyde binder - formaldehyde-free. Even so, the average percentage of fixed carbon in treatment D was slightly lower (63.28%) than the average percentage of fixed carbon in Reference 1 (65.47%).

[00122] Regarding moisture, all treatments showed an average moisture content lower than the References, Petition 870250002351, dated 10 / 01 / 2025, p. 36 / 56 31 / 36 except for treatment D, which showed an average moisture content higher than the references (8.33%).

[00123] For volatiles, the average of all optimized treatments was similar, in the range of 17.32 to 18.83%. All optimized treatments showed an average volatile content lower than the average of the briquettes from Reference 1. Regarding ash content, only treatment D showed an average lower (10.64%) than the average ash percentage of Reference 1. Table 10: Results of the immediate analysis of the optimized briquettes and references, presented as percentages. Formulation Moisture Volatiles Ash Fixed Carbon D 8.33 17.74 10.64 63.28 H 1.57 17.32 14.78 66.34 I 1.00 18.76 13.43 66.80 J 1.50 18.70 13.31 66.49 K 0.90 18.28 14.05 66.77 L 0.95 18.83 12.75 67.48 Reference 1 Reference 2 2.93 6.94 19.29 16.61 12.31 1.94 65.47 74.51 Example 10 - Elemental analysis, higher heating value (HHV) and lower heating value (LHV)

[00124] Table 11 shows the results of the elemental analysis for CHNS-O of the optimized briquettes and References 1 and 2.

[00125] According to Table 11, for elemental carbon content, all optimized briquette treatments (except treatments J and L) showed an average content of Petition 870250002351, dated 10 / 01 / 2025, p. 37 / 56 Treatments J and L showed average carbon content (70.25% and 70.44%, respectively) slightly lower than the average carbon content of the control treatment (70.84%).

[00126] For both nitrogen and hydrogen content, all optimized treatments showed averages similar to the averages of References 1 and 2.

[00127] Regarding sulfur content, in all samples evaluated, both for the optimized briquettes and for the briquettes of the two references, no presence of the element sulfur was detected by the method used.

[00128] Also in Table 11, regarding oxygen content, all optimized treatments (except treatment D free formalin) presented Reference 1. Table 11: Reference CNHS-O contents, presented in percentages (%), showing oxygen content lower than that of the optimized briquettes and the optimized briquettes. Formulation CNHSOD 72.49 0.63 2.18 nd 14.06 H 71.04 1.19 2.79 nd 10.2 I 71.04 1.19 2.79 nd 11.55 J 70.25 1.39 2.83 nd 12.22 K 71.16 1.25 2.8 nd 10.74 L 70.44 1.28 3.2 nd 12.33 Reference 1 70.84 0.83 2.72 nd 13.3 Reference 2 77.68 0.89 2.66 nd 7.32 Petition 870250002351, dated 10 / 01 / 2025, p. 38 / 56 33 / 36

[00129] Table 12, in turn, shows the results for the higher heating value (HHV) and lower heating value (LHV) of the optimized briquettes and the References. Table 12: PCS and PCI of optimized briquettes and reference briquettes. Formulation PCS (Kcal / kg) PCI (Kcal / kg) D 6,625.24 6,510.62 H 6,726.42 6,582.88 I 6,676.23 6,529.53 J 6,629.22 6,480.43 K 6,555.93 6,408.71 L 6,607.71 6,439.46 Reference 1 6,506.93 6,363.92 Reference 2 7,230.22 7,090.36

[00130] According to Table 12, all optimized briquette treatments showed higher higher heating value (HHV) and lower heating value (LHV) than the briquettes from Reference 1. Example 11 - Apparent density analysis

[00131] Table 13 presents the apparent density values ​​of the optimized briquettes and References 1 and 2. Table 13: Apparent density of the optimized briquettes and the reference briquettes. Formulation DA (g / cm3) D 1.08 H 0.98 I 0.97 J 1.01 K 0.99 L 0.99 Reference 1 1.04 Reference 2 1.06 Petition 870250002351, dated 10 / 01 / 2025, p. 39 / 56 34 / 36

[00132] As can be seen in Table 13, for the apparent density variable of the briquettes, the results were similar for all treatments evaluated, both for the optimized briquettes and for the references, remaining in the range of 0.97 to 1.08 g / cm3.

[00133] Only treatment D (formaldehyde-free briquette) showed a higher apparent density (1.08 g / cm3) than the references - briquettes from Reference 1 and briquettes from Reference 2. Example 12: Burning Performance

[00134] Table 14 presents the results of the combustion test of the optimized briquettes and References 1 and 2. Table 14: Burn test results for optimized briquettes and reference briquettes. Formulation 15 min 30 min 45 min 60 min Maximum burning time D 336 Ambient Ambient Ambient 29 min H 550 549 614 411 135 min I 543 553 601 624 170 min J 594 542 611 623 173 min K 595 614 602 526 160 min L 577 622 623 613 145 min Reference 1 578 631 588 602 140 min Reference 2 525 489 590 345 105 min

[00135] According to Table 14, all optimized briquettes (except treatment D - formaldehyde-free) showed a higher maximum firing temperature than the briquettes from Petition 870250002351, dated 10 / 01 / 2025, pp. 40 / 56 35 / 36 Reference 2, for all evaluated burn times - 15, 30, 45 and 60 minutes.

[00136] The optimized briquettes for treatments I, J, and L showed a higher maximum firing temperature than the briquettes from Reference 2, for firing times of 45 and 60 minutes. For firing times of 15 and 30 minutes, the briquettes from treatments I, J, and L showed a slightly lower maximum firing temperature than the briquettes from Reference 1.

[00137] The briquettes from treatment D - formaldehyde-free - showed poor combustion performance, reaching a maximum temperature after 15 minutes of burning, significantly lower than the other optimized briquettes (treatments H to L) and the references. Furthermore, the briquettes from treatment D extinguished after only 29 minutes of burning.

[00138] All optimized briquettes showed a longer total burning time (remained lit and burning for longer) compared to the briquettes from Reference 2. All optimized briquettes showed a longer total burning time (except treatment K) compared to the briquettes from Reference 1.

[00139] Therefore, the briquettes that presented the greatest balance between mechanical, energy and combustion performances were the briquettes from treatment I, with the formulation of 6.5% cassava starch, 6.5% resin containing phenol formaldehyde - FF202 with low emission of free formaldehyde, 2.5% Petition 870250002351, dated 10 / 01 / 2025, pp. 41 / 56 36 / 36 white clay and 0.5% titanium dioxide. And when compared to the briquette formulation of Reference 1, the briquettes of treatment I showed a reduction in production cost, precisely because they require fewer binders than the briquettes of Reference 1. Petition 870250002351, dated 10 / 01 / 2025, pp. 42 / 56

Claims

1 / 3 CLAIMS 1. Production process for standard hookah charcoal briquettes or liturgical charcoal characterized by comprising a mixture of coconut residue and cassava starch (FM), resin containing phenol formaldehyde (FF) with low emission of free formaldehyde and white clay (AB).

2. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 1, characterized by comprising the use of fine vegetable charcoal from babassu coconut residue, composed of epicarp, mesocarp and endocarp, except for the kernels.

3. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 1, characterized by using binders in the following proportions: a. 5 to 12% cassava starch; b. between 0 and 7% resin containing phenol formaldehyde with low emission of free formaldehyde; and c. between 2 and 3.5% white clay.

4. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 1, characterized by using up to 1% titanium dioxide.

5. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 1, characterized by comprising the homogenization of fine vegetable charcoal from babassu coconut residue, Petition 870250002351, dated 10 / 01 / 2025, p. 49 / 56 2 / 3 binders and titanium dioxide and pressing between 350 and 450 bar; 6. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 5, characterized by the pressing of the materials being carried out at 403 bar (40 bar on the pressure gauge); 7. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 1, characterized by the pressing of the materials being carried out between 1 and 20 minutes; 8. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 5, characterized by the pressing of the materials being carried out between 50°C and 100°C; 9. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 8, characterized by the pressing of the materials being carried out between 70°C and 80°C; 10. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to claim 1, characterized in that the briquette, after pressing, is kept at a temperature varying between 70°C and 120°C for between 1 hour and 48 hours.

11. Production process for standard hookah charcoal briquettes or liturgical charcoal, according to Petition 870250002351, dated 10 / 01 / 2025, page 50 / 56 3 / 3, claim 1, characterized by the pressed briquette being kept at a temperature of 105°C for 24 hours.

12. Standard hookah charcoal briquette or liturgical charcoal characterized by its ability to remain lit for more than 150 minutes and at a temperature exceeding 550°C throughout the burning period. Petition 870250002351, dated 10 / 01 / 2025, pp. 51 / 56

Images