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Article

Thermal Processing Effects on on Biomass Ash Utilization for Ceramic Membrane Fabrication

by
Heloísa Maria de Oliveira
,
Hélio de Lucena Lira
* and
Lisiane Navarro de Lima Santana
Department of Science and Materials Engineering, Federal University of Campina Grande, Campina Grande 58400-850, Brazil
*
Author to whom correspondence should be addressed.
Sustainability 2025, 17(3), 979; https://doi.org/10.3390/su17030979
Submission received: 20 December 2024 / Revised: 19 January 2025 / Accepted: 23 January 2025 / Published: 25 January 2025
(This article belongs to the Special Issue Resource Sustainability: Sustainable Materials and Green Engineering)
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Abstract

:
Biomass carbon-rich ash is proposed as a sustainable alternative in the production of ceramic materials. This study investigated this waste product, combined with kaolin and alumina for the production of ceramic membranes. The formulations were defined based on the Al2O3-SiO2-MgO ternary diagram with 51 wt% biomass ash, 36 wt% kaolin, and 13 wt% alumina. The shaping of the green body samples was conducted by using the uniaxial pressing method at 40 MPa and sintering at temperatures ranging from 1050 to 1150 °C. Several properties, such as morphology, porosity, pore diameter, mechanical strength, and chemical resistance, were investigated. It was revealed that the increase in temperature occasioned decreased porosity and water absorption; conversely, it increased bulk density, pore size, diametrical shrinkage, and flexural strength. Moreover, the samples demonstrated minimal weight loss (<0.6 wt.%) in acidic and basic solutions. The samples with porosity ranging from 31.5% to 44.4%, pore size from 1.0 μm to 1.5 μm, and flexural resistance from 9.0 MPa to 21.0 MPa were tested for pure water flux at 1.0 bar and an enhanced flux at a higher temperature, attributed to increased pore size resulting from higher sintering temperatures, was observed. The best-performing sample was sintered at 1050 °C with an average flux of 1716.8 L.h−1.m−2. Also, according to TGA/DTA data, these membranes have greater stability. These membranes are suitable for the treatment of effluents and contribute to reducing environmental impact and increasing sustainability by promoting the efficient utilization of resources.

1. Introduction

Reducing dependence on fossil fuels and mitigating greenhouse gas emissions is a sustainable strategy and necessitates the adoption of renewable energy sources like biomass. Currently, biomass contributes approximately 10% of the global energy mix, with projections estimating a growth of 30% by 2030 [1]. However, the increasing industrial use of biomass as an energy source has led to higher production of biomass ash (BA), an inorganic byproduct of combustion. Composed mainly of alkaline and alkaline-earth metals, silica, and sulfur, BA presents significant environmental risks when improperly disposed of, as its fine particles can cause respiratory issues and contaminate soil, groundwater, and air [2,3].
The composition, quantity, and properties of ashes vary based on the combusted feedstock, such as eucalyptus wood or grain husks, as well as the industrial waste and combustion efficiency. For example, black ash indicates unburned carbon, while light gray ash reflects higher combustion efficiency and reduced carbon content. The high levels of unburned carbon are linked to incomplete combustion and the low melting temperatures of biomass, resulting in larger ash volumes [4].
The use of biomass ash in the manufacturing of ceramic membranes is studied by some researchers [5,6,7]. Generally, the solid waste selected for the production of membranes has high levels of alumina, silica, zirconia or titanium titania [7,8]. However, the presence of low-melting-point oxides can significantly influence the temperature required for sintering. In addition, the presence of unburned carbon ash can affect several aspects of the performance of ceramic membranes, such as strength, porosity, permeability, and separation capacity [7].
Usually, the high content of silica and alumina in ashes is particularly suitable for the formulation of ceramic materials. Its incorporation into ceramic masses can enhance physical and mechanical properties, including mechanical strength, hydrophilicity, and thermal stability [4]. Moreover, biomass ashes have been classified into four chemical types (S, C, K, and CK), further subdivided into three categories based on acidity (high, medium, or low) [9]. This classification depends on the characteristics of the minerals present, categorized as detrital or authigenic. Detrital minerals, such as silicates and oxyhydroxides, are stable, less mobile, and have high melting points. In contrast, authigenic minerals, such as opals, carbonates, sulfates, and nitrates, are more reactive, mobile, and unstable, with low decomposition temperatures.
This mineralogical diversity offers both fundamental and practical opportunities. The distinct properties of BA can be tailored for specific industrial applications, such as producing advanced ceramics or ceramic membranes for water and waste treatment. Unlike coal ash, the variable inorganic composition of biomass ash allows for greater flexibility in material design. Thermal treatment can further refine the structure and composition of ash to meet targeted application requirements [4].
Given the high costs of synthetic raw materials, economically viable alternatives such as natural minerals (e.g., kaolin, bauxite, diatomite), solid waste, and BA have garnered interest. These materials serve as raw inputs for ceramic membrane production, acting as structural supports, selective layers, or even sintering additives, thereby reducing production costs [8]. However, a key challenge in using these materials for ceramic membranes lies in the variability of their chemical compositions. The accurate characterization of BA is critical, as its properties differ significantly depending on the feedstock and combustion process. Low-melting-point oxides of biomass waste can influence sintering temperatures, while unburned carbon may impact the membrane’s strength, porosity, permeability, and separation efficiency [7].
While several studies have explored the use of biomass waste in ceramic membranes [6,10,11,12,13,14,15,16,17], no studies in the literature have addressed the use of BA derived from eucalyptus, cashew nut shells, babassu coconut, or mesquite. This study aims to address this gap by reusing natural and calcined biomass ashes (BA and CBA, respectively) as a sustainable alternative material in the fabrication of ceramic membranes, combined with kaolin and alumina. This study also investigated properties such as flexural strength, porosity, pore size, diametrical shrinkage, chemical resistance, and water flux to identify potential applications.

2. Materials and Methods

2.1. Raw Materials and Characterization

The biomass ash (BA), shown as Figure 1, derived from eucalyptus, babassu coconut, cashew nutshell, and mesquite, was provided by the mining industry from Brazil. Kaolin was obtained from Rocha Minérios (Caetité, Bahia, Brazil) and alumina was from Imerys (Salto, São Paulo, Brazil).
The BA was processed using a Servitech roller mill for 1 h and a Servitech CT-242 jar mill for 30 min (Servitech Equipamentos Industriais, Tubarão, Brazil). The calcinated biomass ash, called CBA, was subjected to heat treatment with temperatures ranging from room temperature to 700 °C, with a plateau of 1 h and a heating rate of 5 °C.min⁻1. The raw materials were characterized by chemical analysis on a Shimadzu EDX-720 vacuum system (Shimadzu, Barueri, Brazil) to identify the metallic oxides. Particle size analysis was performed using a wet method using a Cilas laser granulometer, model 1064 (Cilas, Orléans, France). Figure 2 shows BA after beneficiation and thermal treatment.

2.2. Membrane Preparation

In this study, the formulations were defined based on the chemical analysis of raw materials. The ceramic masses were homogenized using a ball mill Servitech at 300 RPM for 24 h, refined through an ABNT 200 sieve (0.075 mm), and subjected to the chemical analysis. Furthermore, the ceramic masses were moistened with distilled water at ~10% and shaped using the uniaxial pressing method with the aid of a Bovenau hydraulic press for flat disk samples (30 mm × 3 mm) and a Servitech hydraulic press for rectangular samples (50 mm × 15 mm × 5 mm), both at 40 MPa. The rectangular samples were made exclusively for mechanical strength testing. Subsequently, the samples were dried in a Fanem 515-A oven (Fanem, Guarulhos, Brazil) at 110 °C for 24 h to remove the moisture and sintered in an Inti Maitec furnace (Maitec, São Carlos, Brazil) at three temperatures, starting with an initial plateau at 500 °C for 1 h (to remove the organic matter and impurities) and a heating rate of 2 °C.min⁻1, and the final temperatures were 1050 °C, 1100 °C, and 1150 °C with a plateau for 1 h and a heating rate of 5 °C.min⁻1. Figure 3 presents a flowchart describing the process of preparing ceramic membranes and the analyses performed.

Characterization

To identify the crystalline structures and phase transformations, a Shimadzu XDR-6000 diffractometer (Shimadzu, Barueri, Brazil) was used, employing Cu Kα radiation (40 kV/30 mA). The structural parameters of sintered samples were assessed by the Rietveld refinement of the XRD data using the RITA/RISTA routine from software program materials analysis using diffraction (MAUD) version 2.996 [18,19]. The diametrical shrinkage was measured using a vernier caliper (Digimess). Apparent porosity, water absorption and bulk density were determined using the Archimedean method, using water as fluid. The mercury intrusion porosimetry technique was used for analyzing the pore size distribution with Micrometrics AutoPore IV 9500 V1.09 (Micromeritics, Norcross, GA, USA). The three-point bending test was realized using a universal testing machine Shimadzu Autograph AGX (Shimadzu, Barueri, Brazil) to determine the flexural strength, with a maximum load of 50 KN and a loading speed of 0.5 mm/min.
Scanning electron microscopy was employed to evaluate the microstructure of the ceramic membranes in the fracture section. A Tescan Vega3 (Tescan, Sao Bernardo do Campo, Brazil) scanning electron microscope was used, operating in secondary electron mode at a voltage of 20 kV.
The chemical corrosion resistance of the ceramic membranes was evaluated based on mass loss after being subjected to acidic HCl 0.1 M (pH = 1.5) and alkaline NaOH 1 M solutions (pH = 13.0) at room temperature for 7 days [20].
The tangential pure water flux through the ceramic membranes was obtained using Equation (1), where JW is the pure water flux (L.m−2.h−1), Q is the amount of permeate water (L), A is the membrane area (m2), and Δt is the time interval (h).
J W = Q A × ∆ t

3. Results

The chemical composition (Table 1) of the raw materials indicates that the main constituent of BA and CBA is SiO2 (67.3% and 51.1%, respectively). The MgO present can be attributed to the presence of cashew nutshell [20,21] and leaks occurring during the calcination of magnesite in the industry. The presence of alkali oxides such as K2O, MgO, CaO, and Fe2O3 can reduce the melting temperature and promote the formation of the liquid phase. The LOI in BA (22.9%) can be attributed to the removal of organic matter.
Kaolin contains basically SiO2 (52.6%) and Al2O3 (45.5%), with a SiO2/Al2O3 ratio of 1.1, in addition to trace amounts of K2O, Fe2O3, and other oxides. Alumina indicates high purity (99.9% Al2O3).
The granulometry results are presented in Figure 4. The calcined biomass (Figure 4a) presented approximately 19% of particles with a particle diameter <10 μm and 80% of particles with a diameter <65 μm. Regarding kaolin (Figure 4b), 80% of the particles had a diameter <10 μm, and alumina (Figure 4c) had 80% of the particles with a diameter <5 μm.
The classification of BA and CBA in the chemical system of inorganic matter in biomass and biomass ashes (5) categorizes them as “S”-type materials, with BA located in the high acid (HA) region and CBA located in the medium acid (MA) region. Potential applications for BA, based in the S-HA classification, include adsorbents, bricks, catalysis, ceramics, concrete, insulators, pavements, reactive pozzolanas, and geopolymer synthesis. For CBA, classified as S-MA, possible applications include bricks, ceramics, concrete, pavements, pozzolanas, and geopolymer synthesis [9]. Thus, both BA and CBA exhibit characteristics suitable for ceramic applications.
Correlating the chemical analysis of raw materials with the Al2O3-SiO2-MgO ternary diagram, such as Figure 5, and to add value to the biomass ash, the following formulation was defined: 51% biomass ashes, 36% kaolin, and 13% alumina, denominated of FCA and FCBA, for the formulation with natural and calcined BA, respectively.
The chemical composition of the FBA and FCBA, mentioned in Table 2, highlights the predominance of SiO2, Al2O3, and MgO, in accordance with ternary diagram.
The TGA-DTA curves for the mass formulations are shown in Figure 4. For FBA (Figure 6a), three main mass loss events are identified. The first occurred up to ~320 °C, where a mass loss of 8.1% was observed, associated with the removal of adsorbed water and the predehydroxylation of kaolinite [22]. The second mass loss took place between ~320 °C and 730 °C, with a mass reduction of 20.0%, characterized by an exothermic peak at around ~425.6 °C, attributed to the deydroxylation of kaolinite [22] and the combustion of organic matter associated with the BA [23]. These results, attributed to the presence of kaolinite, are confirmed by XRD in Figure 7. The final mass loss happened between ~730 °C and 1000 °C, with a mass loss of 4.4%, which can be attributed to the residual removal of hydroxyl groups [22] and the burning of some residual char associated with BA [23]. The total mass loss at 1000 °C amounted to 32.5%. The low mass loss temperature highlighted the BA as a potential candidate to be used as a pore-forming agent in the preparation of low-cost ceramic membranes.
For FCBA (Figure 6b), three main mass loss events were also identified. The first occurred between ~230 °C and 416 °C, with a weight loss of 0.4%, likely associated with the loss of adsorbed water and the predehydroxylation of kaolinite [22]. The second mass loss took place between ~416 °C and 730 °C, with a mass reduction of 3.9%, corresponding to the deydroxylation of kaolinite [22]. The last mass loss happened between ~730 °C and 1000 °C, with a mass reduction of 2.8%, associated with the residual removal of hydroxyl groups [22]. The total mass loss at 1000 °C amounted to 7.1%.
Figure 7 presents the XRD patterns of formulations before and after thermal treatment. The mineralogical analysis for FBA and FCBA before the sintering presents characteristic peaks of quartz (ICSD 034636) [24], periclase (ICSD 061325) [25], kaolinite (ICSD 080082) [26], and corundum (ICSD 088028) [27].
For FBA (Figure 7a) and FCBA (Figure 7b) after sintering, mineralogical analysis reveals characteristic peaks of quartz (ICSD 034636), cristobalite (ICSD 047220) [28], corundum (ICSD 088028), forsterite (ICSD 026374) [29], mullite (ICSD 066448) [30], and periclase (ICSD 061325) at 1050 °C and 1100 °C. At 1150 °C, a reduction in the intensity of the quartz, corundum, forsterite, and mullite peaks was noted, and spinel (ICSD 079000) [31] and cordierite (ICSD 202174) [32] peaks appeared.
At 1050 °C, low-intensity mullite peaks appear. Although mullite typically forms at higher temperatures (>1200 °C), the presence of fluxing oxides facilitates its early nucleation and crystallization. For the Al2O3–SiO2 binary system, the liquid-phase formation occurs at 1595 °C. However, in the Al2O3–SiO2–K2O ternary system, this temperature is significantly reduced to 985 °C. The presence of other impurity oxides can further lower the onset of liquid-phase formation [33].
Low-intensity peaks of forsterite also are observed at 1050 °C. Between 830 and 860 °C, forsterite may begin to form, possibly through two reactions: the direct reaction between SiO2 and MgO, or a two-step reaction, where the initial interaction of SiO2 and MgO forms enstatite, which then reacts with MgO to produce forsterite [34]. Since no characteristic enstatite peaks were observed in the XRD of the samples, forsterite may have formed through the direct reaction, or all enstatite formed during the process could have been converted into forsterite.
At 1150 °C, periclase reacts with corundum to form spinel. Magnesium aluminate spinel is primarily formed in the range of 900–1200 °C and totally above 1300 °C, depending on precursor reactivity and synthesis conditions. The presence of fluxing oxides likely promotes a liquid-phase formation that facilitates ion diffusion, accelerates the reaction, and enables spinel crystallization [35]. Moreover, the mullite phase can react with magnesium oxide at 1150 °C to form spinel and cordierite [36].
Table 3 shows the results of Rietveld refinement of FBA and FCBA sintered at 1050 to 1150 °C. The samples were refined using the ICSD database. The ICSD cards nº 034636, 047220, 088028, 026374, 066448, 061325, 079000, and 202174 are applied to identify, respectively, quartz, cristobalite, corundum, forsterite, mullite, periclase, spinel, and cordierite crystalline phases. Based on the refinement data obtained, the concordance factors for the refinements of the standard samples and with residue content were in the ranges of Rwp of ~19.6 to 16.3 and Rexp of ~9.1 to 9.14 (See Table 3). The goodness-of-fit (χ2) values were relatively low, meaning all were approximately 2%, which is an indication of the good quality of the refinements [37].
Table 4 summarizes the apparent porosity, water absorption, bulk density, diametrical shrinkage, flexural strength, and chemical resistance for FBA and FCBA. FBA exhibited higher porosity and water absorption, but a lower bulk density than FCBA for all temperatures. This behavior may be related to the organic matter present in FBA, which acts as a pore-forming agent. Porosity decreased from 44.4% to 22.7% for FBA and from 31.5% to 5.7% for FCBA with increasing temperature from 1050 °C to 1150 °C, respectively. The increase in temperature is accompanied by densification, and then the formation of the glassy phase, which increases sinterability, may fill the porosity or close it. This phenomenon leads to the decreasing of the support porosities. Similar behavior was observed by others researchers [38,39,40,41]. For the same reason, water absorption decreases from 27.3% to 10.9% for FBA and from 15.9% to 2.2% for FCBA when the temperature increases from 1050 °C to 1150 °C, respectively.
Diametrical shrinkage and flexural strength increased, from 2.9% to 10.3% for FBA and from 2.7% to 10.3% for FCBA, and from 9.0 MPa to 30.0 MPa for FBA and from 21.0 MPa to 51.8 MPa for FCBA, respectively, with temperature for both compositions increased from 1050 °C to 1150 °C, also associated with liquid-phase formations and particle rearrangement. The formation of new phases, such as mullite and spinel, is presumed to contribute to enhanced flexural strength [35,42].
During the chemical cleaning process, membranes are typically immersed in solutions containing either acidic or basic chemicals. Therefore, conducting a chemical resistance test is crucial to evaluating the sample’s behavior against chemical corrosion, ensuring its durability and performance under various operational conditions [43]. The results of chemical resistance tests, given in Table 4, reveal that the samples undergo minimal weight loss in both acidic and basic mediums (less than 0.6 wt.%), thus signifying the promising suitability for use in harsh acidic and basic conditions.
The distribution of the pore sizes for FBA and FCBA was observed in Figure 8. For the FBA, increasing the temperature from 1050 °C to 1150 °C resulted in an increase in average pore size from 1.5 μm to 3.1 μm. According to researchers [44], the reduction in the viscosity of the liquid phase during sintering, which is formed by the existence of fluxing oxides, favors the filling of pores. Increasing the sintering temperature stimulates pore coalescence, favoring an increase in the average pore diameter. In accordance with [45], this may occur because during the heating process, the formation of a liquid phase promotes its migration into smaller pores between solid particles, driven by capillary forces. This phenomenon facilitates the elimination of smaller pores, contributing to the growth of larger pores [41,46,47]. For FCBA, an increase in the average pore size from 1.0 μm to 1.3 μm was observed when the temperature was raised from 1050 °C to 1100 °C; however, at 1150 °C, the average pore size decreased to 1.0 μm. This behavior can be attributed to higher densification of FCBA, resulting from the formation of a liquid phase [48] and a crystalline spinel phase. As the CBA used in this composition had undergone thermal treatment, this led to the volatilization of the organic matter that would otherwise act as a pore-forming agent. Regarding pore-size related applications, all samples are classified for microfiltration, as their average pore sizes fall within the range from 0.1 to 10 μm [49].
Figure 9 presents the SEM images showing the distribution of pores in the fracture of FBA and FCBA sintered at 1050 °C, 1100 °C and 1150 °C. For FBA, an increase in pore size with temperature was observed, as indicated by porosimetry results. For FCBA, the pore size increased when the temperature was raised from 1050 °C to 1100 °C, like the behavior of FBA. When the temperature increased to 1150 °C, the pore size decreased due to the densification of samples, which also reflected in the increase in bulk density previously mentioned.
The samples FBA 1050 °C (44.4% porosity, 1.5 μm pore size, and 9.0 MPa), FBA 1100 °C (36.1% porosity, 2.4 μm pore size, and 17.3 MPa), and FCBA 1050 °C (31.5% porosity, 1.0 μm pore size, and 21.0 MPa) were chosen for the water flux tests due to their higher porosity and narrower pore size distribution, which are expected to result in better selectivity during the filtration process. The pure water flux at 1 bar for these membranes is shown in Figure 10. The average flux for FBA 1050 °C was 1921.0 L.h−1.m−2, for FBA 1100 °C, it was 2228.4 L.h−1.m−2, and for FCBA 1050 °C, it was 1716.8 L.h−1.m−2. After 40 min, the flux stabilized. The membrane sintered at a higher temperature (FBA 1100 °C) demonstrates enhanced water flux, which can be attributed to increased pore size resulting from higher sintering temperatures [50].
Based on the results presented in this study, considering the porosity, pore size, and mechanical strength data, FBA 1050, FBA 1100, and FCBA 1050 exhibit potential for various applications, such as textile effluent treatment, tannery wastewater, domestic wastewater, and oil–water emulsions [43,51,52].
Based on the results presented in this study and in Table 5, considering the porosity, pore size, and mechanical strength data, FBA 1050, FBA 1100, and FCBA 1050 exhibit potential for various applications, such as textile effluent treatment, tannery wastewater, domestic wastewater, and oil–water emulsions.

4. Conclusions

This study demonstrated the feasibility of using biomass ash as a sustainable alternative material combined with kaolin and alumina to produce ceramic membranes.
The biomass has a composition rich in SiO2, Al2O3, and MgO, in addition to a significant amount of fluxing oxides, which probably contributed to the densification of the test specimens at higher temperatures.
After thermal treatment, the formulations contained SiO2, Al2O3, and MgO oxides, and presented mullite and forsterite at 1050 °C and 1100 °C, while spinel and cordierite were additionally formed at 1150 °C.
The increase in temperature resulted in a reduction in apparent porosity and water absorption, in addition to increasing the apparent specific mass, linear shrinkage, and flexural strength. These effects are probably related to the formation of a glassy phase and phase transformations.
The increase in temperature caused a variation in pore sizes, with an increase followed by a decrease, as observed by the results of mercury porosimetry and scanning electron microscopy (SEM) images.
All samples exhibited minimal mass loss in acidic and basic solutions (<0.6 wt.%), demonstrating excellent chemical resistance.
The best properties for membranes with natural biomass ash were achieved at sintering temperatures of 1050 °C and 1100 °C, with porosity values of 44.4% and 36.1%, average pore sizes of 1.5 μm and 2.4 μm, mechanical strengths of 9.0 MPa and 17.3 MPa, and average water fluxes of 1921.0 L.h−1.m−2 and 2228.4 L.h−1.m−2, respectively.
For calcined biomass ash, the best-performing sample was sintered at 1050 °C, with a porosity of 31.5%, an average pore size of 1.0 μm, a mechanical strength of 21.0 MPa, and an average flux of 1716.8 L.h−1.m−2. Also, according to TGA/DTA data, these membranes have greater stability.
These membranes are classified as suitable for microfiltration and exhibit potential for the treatment of effluents such as wastewater from the textile and tannery industries and oil–water emulsions and contribute in this way to reducing environmental impact and increasing sustainability by promoting the efficient utilization of resources.

Author Contributions

Methodology, software, formal analysis, investigation, data curation, writing—original draft preparation, and writing—review, H.M.d.O.; conceptualization, writing—review, editing, supervision, project administration, resources, and funding acquisition, H.d.L.L. and L.N.d.L.S. All authors have read and agreed to the published version of the manuscript.

Funding

This research was funded by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES), grant number 88887.911998/2023-00.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

All data presented in this study are available on request from the corresponding author.

Acknowledgments

The authors are grateful to CAPES for financial assistance.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. BA derived from the use of biomass as an energy source.
Figure 1. BA derived from the use of biomass as an energy source.
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Figure 2. (a) BA after the beneficiation process and (b) thermally treated CBA.
Figure 2. (a) BA after the beneficiation process and (b) thermally treated CBA.
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Figure 3. Process of preparing ceramic membranes and the analyses performed.
Figure 3. Process of preparing ceramic membranes and the analyses performed.
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Figure 4. Granulometry for (a) CBA, (b) kaolin, and (c) alumina.
Figure 4. Granulometry for (a) CBA, (b) kaolin, and (c) alumina.
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Figure 5. MgO-Al2O3-SiO2 phase equilibrium diagram [adapted from [21]]. ●FBA formulation with natural BA and ●FCBA formulation with calcined BA.
Figure 5. MgO-Al2O3-SiO2 phase equilibrium diagram [adapted from [21]]. ●FBA formulation with natural BA and ●FCBA formulation with calcined BA.
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Figure 6. TGA and DTA for (a) FBA and (b) FCBA.
Figure 6. TGA and DTA for (a) FBA and (b) FCBA.
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Figure 7. XDR for (a) FBA and (b) FCBA before and after thermal treatment (◄—kaolinite; ●—quartz; ▲—corundum; ○—periclase; ♣—cordierite; ■—mullite; ◊—spinel; □—cristobalite; ♠—forsterite).
Figure 7. XDR for (a) FBA and (b) FCBA before and after thermal treatment (◄—kaolinite; ●—quartz; ▲—corundum; ○—periclase; ♣—cordierite; ■—mullite; ◊—spinel; □—cristobalite; ♠—forsterite).
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Figure 8. Pore size distribution for (a) FBA 1050 °C, (b) FBA 1100 °C, (c) FBA 1150 °C, (d) FCBA 1050 °C, (e) FCBA 1100 °C, and (f) FCBA 1150 °C.
Figure 8. Pore size distribution for (a) FBA 1050 °C, (b) FBA 1100 °C, (c) FBA 1150 °C, (d) FCBA 1050 °C, (e) FCBA 1100 °C, and (f) FCBA 1150 °C.
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Figure 9. SEM images in the fracture section for (a) FBA 1050 °C; (b) FBA 1100 °C; (c) FBA 1150 °C; (d) FCBA 1050 °C; (e) FCBA 1100 °C; (f) FCBA 1150 °C.
Figure 9. SEM images in the fracture section for (a) FBA 1050 °C; (b) FBA 1100 °C; (c) FBA 1150 °C; (d) FCBA 1050 °C; (e) FCBA 1100 °C; (f) FCBA 1150 °C.
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Figure 10. Pure water flux at 1.0 bar for FBA 1050, FBA 1100, and FCBA 1050.
Figure 10. Pure water flux at 1.0 bar for FBA 1050, FBA 1100, and FCBA 1050.
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Table 1. Chemical compositions of raw materials.
Table 1. Chemical compositions of raw materials.
SampleSiO2MgOAl2O3K2OFe2O3CaOP2O5OthersLOI *
BA (%)67.312.36.95. 13.92.11.11.222.9
CBA (%)51.121.68.66.85.93.71.81.1-
Kaolin (%)52.6-45.50.90.6--0.1-
Alumina (%) -99.9----0.1-
* LOI—Loss on Ignition at 1000 °C.
Table 2. Chemical compositions of formulations of FBA and FCBA.
Table 2. Chemical compositions of formulations of FBA and FCBA.
SampleSiO2MgOAl2O3K2OFe2O3CaOP2O5Others
FBA (%)50.75.336.13.62.01.10.50.7
FCBA (%)47.77.237.52.92.21.40.60.5
Table 3. Results for Rietveld refinement.
Table 3. Results for Rietveld refinement.
SampleFBA 1050FBA 1100FBA1150FCBA 1050FCBA 1100FCBA 1150
RWP (R-weighted profile)16.419.517.116.319.617.4
REXP (R-expected)9.39.19.19.49.29.4
χ2 (Goodness of fit) 1.82.11.91.72.11.8
PhaseWeight (%)
Quartz
(hexagonal)		42.840.533.445.844.927.7
Corundum
(rhombohedral)		34.937.428.231.636.726.6
Spinel
(cubic)		--19.1--33.1
Mullite
(orthorhombic)		9.511.09.38.25.62.0
Periclase
(cubic)		5.53.83.15.04.22.6
Cristobalite
(tetragonal)		1.72.12.01.82.11.9
Forsterite
(orthorhombic)		5.85.24.27.66.54.8
Cordierite
(orthorhombic)		--0.8--1.3
Table 4. Apparent porosity, water absorption, bulk density, diametrical shrinkage, flexural strength, and chemical resistance for all specimens.
Table 4. Apparent porosity, water absorption, bulk density, diametrical shrinkage, flexural strength, and chemical resistance for all specimens.
SampleFBA 1050FBA 1100FBA1150FCBA 1050FCBA 1100FCBA 1150
Apparent
porosity (%)		44.4 ± 0.336.1 ± 0.322.7 ± 0.531.5 ± 0.523.4 ± 0.65.7 ± 0.5
Water
absorption (%) 		27.3 ± 0.220.0 ± 0.210.9 ± 0.215.9 ± 0.310.6 ± 0.42.2 ± 0.2
Bulk
density (a.u.)		1.6 ± 0.01.8 ± 0.02.1 ± 0.02.0 ± 0.02.2 ± 0.02.6 ± 0.0
Diametrical shrinkage (%)2.9 ± 0.06.0 ± 0.110.3 ± 0.12.7 ± 0.16.4 ± 0.110.3 ± 0.2
Flexural strength (MPa)9.0 ± 0.217.3 ± 0.630.0 ± 1.421.0 ± 0.634.9 ± 1.451.8 ± 2.2
Chemical resistance
Weight loss in acid (%)0.1 ± 0.20.5 ± 0.30.2 ± 0.20.1 ± 0.10.2 ± 0.30.4 ± 0.2
Weight loss in base (%)0.1 ± 0.20.1 ± 0.20.5 ± 0.20.5 ± 0.30.2 ± 0.30.2 ± 0.2
Table 5. Potential applications for FBA 1050, FBA 1100, and FCBA 1050 based on studies in the literature.
Table 5. Potential applications for FBA 1050, FBA 1100, and FCBA 1050 based on studies in the literature.
Raw
Materials		Sintering
Temperature (°C)		Porosity (%) Pore Size (μm)Mechanical Strength (MPa)ApplicationEfficiency (%)Reference
Kaolin, quartz, calcium carbonate90030.01.334.0Oil-in-water emulsions82.0[50]
Natural clay magnesite110047.01.16.1Industrial textile wastewater99.0[51]
Ball clay, quartzite waste, and starch100035.01.38.6Domestic laundry wastewater91.0[42]
Natural clay, starch, and SiO295043.01.432.0Tannery effluent
Textile wastewater		99.3
98.2		[52]
FBA, kaolin, and alumina1050
1100		44.4
36.1		1.5
2.4		9.0
17.3		--This work
FCBA, kaolin, and alumina105031.51.021.0--This work
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de Oliveira, H.M.; de Lucena Lira, H.; de Lima Santana, L.N. Thermal Processing Effects on on Biomass Ash Utilization for Ceramic Membrane Fabrication. Sustainability 2025, 17, 979. https://doi.org/10.3390/su17030979

AMA Style

de Oliveira HM, de Lucena Lira H, de Lima Santana LN. Thermal Processing Effects on on Biomass Ash Utilization for Ceramic Membrane Fabrication. Sustainability. 2025; 17(3):979. https://doi.org/10.3390/su17030979

Chicago/Turabian Style

de Oliveira, Heloísa Maria, Hélio de Lucena Lira, and Lisiane Navarro de Lima Santana. 2025. "Thermal Processing Effects on on Biomass Ash Utilization for Ceramic Membrane Fabrication" Sustainability 17, no. 3: 979. https://doi.org/10.3390/su17030979

APA Style

de Oliveira, H. M., de Lucena Lira, H., & de Lima Santana, L. N. (2025). Thermal Processing Effects on on Biomass Ash Utilization for Ceramic Membrane Fabrication. Sustainability, 17(3), 979. https://doi.org/10.3390/su17030979

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