Superacid Sites Research Articles

Production of biodiesel from waste culinary oil catalyzed by S2O82−/TiO2–SiO2 solid super-acid catalyst prepared with recovered TiO2 from spent SCR

Recovery and valorization of natural resources from waste materials are crucial for promoting sustainable development. In light of this, the present study explores the transesterification of waste culinary oil into biodiesel production using a silica-supported solid super-acid catalyst (S2O82−/TiO2–SiO2) prepared with recovered TiO2 from spent SCR. The synthesized materials were characterized through XRD, SEM-DES, XPS, FT-IR, NH3-TPD, and N2-BET analysis. Notably, the crystal structure of recovered TiO2 was not destroyed during the whole process. N2-BET analysis showed that the silica-supported catalyst significantly increased the specific surface area from 47.89 to 101.16 g/m2. The presence of superacid sites (Brønsted and Lewis acid sites) on the surface of the catalyst was confirmed by NH3-TPD and FT-IR analysis. The silica-supported catalyst (S2O82−/TiO2–SiO2) exhibited high catalytic activity for free fatty acid (FFA) about a conversion rate of 90.7 % under optimal reaction conditions: a reaction time of 4 h, at 180 °C with a 5 wt% catalyst loading, and a methanol-to-oil molar ratio of 12:1. The biodiesel production was confirmed by using FT-IR and 1HNMR techniques. Furthermore, the catalytic performance of the prepared catalyst was compared with other catalysts prepared from pure TiO2 reported in the literature. This approach showed a potential for sustainable biodiesel production by using low-cost solid acid catalyst synthesized from recovered materials.

Accurate Measurements of NH3 Differential Adsorption Heat Unveil Structural Sensitivity of Brønsted Acid and Brønsted/Lewis Acid Synergy in Zeolites.

Differential adsorption heats of NH3 on a series of zeolites, including MOR, MFI, FER, and BEA, are accurately measured to probe their acidity using flow-pulse adsorption microcalorimetry. Initial adsorption heats of NH3 at Brønsted acid sites (BAS) vary between 105 to 136 kJ/mol, depending on framework aluminum amounts and topography structures of zeolites. A Brønsted/Lewis acid synergy between BAS and proximate tricoordinated framework-associated aluminum species is identified to generate super acid sites with initial adsorption heats of NH3 around 150 kJ/mol, but occurs only in the MFI zeolites and sensitively depends on the Si/Al ratio. These accurate data of NH3 differential adsorption heats unveil structural sensitivity of BAS and Brønsted/Lewis acid synergy in zeolites and provide experimental benchmark data for fundamental understanding of acidity and acid-catalysis of zeolites.

Persica Akhani Salicornia as novel biodiesel feedstock production for economic prosperity in salty and water scarcity areas: Optimized oil extraction process and transesterification reaction using new magnetic heterogenous nanocatalysts

As a new biodiesel feedstock, the oil extraction procedure from the seeds of the plant Salicornia (Persica Akhani subspecies) has been developed. Oil extraction from the seeds of the Salicornia Persica Akhani has been researched utilizing two different organic solvents and four different procedures, including the Soxhlet method, the traditional approach, the shaker method, and the ultrasonic probe method. The results indicated that oil yield by ultrasonic probe technique was higher than the other methods in a short time. Based on the outcomes, extracting the oil from Salicornia seeds using hexane resulted in a greater yield of oil than petroleum ether. This was true across all methods of extraction. The Physico-chemical properties and antioxidant activity of extracted oil suggested its suitability for biodiesel production. To transesterification reaction of Salicornia seeds oil with methanol into biodiesel, the heterogeneous magnetic Zn0.4Ni0.6Fe2O4 and Zn0.4Ni0.6Fe2O4@SO3H nanocomposites have been synthesized by sol-gel auto combustion procedure. FT-IR, FE-SEM, EDS, and VSM were used to determine the characteristics of the heterogeneous nanocomposites. These nanoparticles have a strong attraction to an outside magnet, which makes it much easier to collect them from the reaction environment for subsequent reuse. In the process of transesterification of Salicornia oil with methanol, novel sulfonated heterogeneous magnetic catalysts with a high density of superacid sites on the surface (2.50 mmol SO3H g−1) and significant magnetization (60 emu/g) afforded high activity and produced a biodiesel yield of 96%. In addition, the magnetic Zn0.4Ni0.6Fe2O4@SO3H nanoparticles could be reused up to five times in the process of turning oil into biodiesel, which resulted in reduced expenses associated with the manufacture of biodiesel. FT-IR and SEM analyses were performed both before and after the transesterification process, and the results showed that the absorption bands and particle distribution were practically the same in both new and used catalysts. The analysis of the FT-IR spectra reveals indications of the transformation of Salicornia oil into fatty acid methyl esters (FAMEs). Gas chromatography (GC) study of the FAME profiles of the as-prepared biodiesel also indicated that palmitic acid (C16:0) was the most saturated fatty acid (8.44%–8.50%), while linoleic acid (18:2) was the predominant unsaturated fatty acid (60.94%–60.97%).

Ru single-atom catalyst anchored on sulfated zirconia for direct methane conversion to methanol

The direct CH4 conversion (DMC) to methanol is a challenging topic. In this study, the Ru/SZ (sulfated zirconia) single-atom catalysts (SACs) were synthesized and utilized to the DMC to methanol under mild conditions (70 °C). The yield over the Ru/SZ SACs (18.32 µmol, TOF ≥ 80 h–1) significantly exceeded the sum of the yields over the SZ (0.67 µmol) and Ru/ZrO2 (0.29 µmol), indicating that a new active center was formed on the Ru/SZ SACs. Combined with the results of the 13CH4 isotope labeling experiments and various characterizations including the pyridine adsorption infrared spectroscopy, electron paramagnetic resonance and X-ray photoelectron spectroscopy, an unprecedented synergy effect between the single-atom and the super acid sites was pictured: The strong acidity of the Ru/SZ SACs could effectively promote the decomposition of H2O2 into the •OH, and the Ruδ+ (δ > 4) and the adjacent Zrγ+-•OH (γ > 4) could synergistically catalyze the CH4 to methanol.

Developing ordered mesoporous silica superacids for high-precision adsorption and separation of ammonia

NH3 reversible adsorption and separation show great significance during its production and utilization, traditional adsorbents show either complex synthetic procedures or unsatisfied separation precision. We report here a class of sulfonic group functionalized and ordered mesoporous silica superacids (OMS-SO3H-xs) via enhanced host–guest assembly between copolymer templates and silica precursors without additional solvent. The OMS-SO3H-xs have large surface areas (463.7–910.5 m2/g), abundant micropores tandem well-ordered mesopores, high concentration of –SO3H (2.5 mmol/g) with extremely-high acid strength. Consequently, the OMS-SO3H-xs exhibit ultra-high precision for NH3 reversible adsorption and separation, giving high NH3 capacity (9.0 & 7.6 mmol/g at 25 & 50 °C and 1.0 bar) with extraordinary NH3/N2 (0.1/0.9) Ideal Adsorption Solution Theory (IAST) selectivities (1200 & 2235). The room temperature saturated breakthrough NH3 capacities of OMS-SO3H-xs were up to 3.38 mmol/g (3.0v%NH3/24.75v%N2/72.25v%H2), which can be well-maintained after 8th cycling without attenuation. The above features found in the OMS-SO3H-xs were resulted from their high density of –SO3H superacid sites those were homogeneously anchored into the ordered mesoporosity, which not only enhances their interaction with NH3, but also achieves the controllable NH3 interaction and transportation inside the mesochannels.

Engineered assembly of water-dispersible nanocatalysts enables low-cost and green CO2 capture

Catalytic solvent regeneration has attracted broad interest owing to its potential to reduce energy consumption in CO2 separation, enabling industry to achieve emission reduction targets of the Paris Climate Accord. Despite recent advances, the development of engineered acidic nanocatalysts with unique characteristics remains a challenge. Herein, we establish a strategy to tailor the physicochemical properties of metal-organic frameworks (MOFs) for the synthesis of water-dispersible core-shell nanocatalysts with ease of use. We demonstrate that functionalized nanoclusters (Fe3O4-COOH) effectively induce missing-linker deficiencies and fabricate mesoporosity during the self-assembly of MOFs. Superacid sites are created by introducing chelating sulfates on the uncoordinated metal clusters, providing high proton donation capability. The obtained nanomaterials drastically reduce the energy consumption of CO2 capture by 44.7% using only 0.1 wt.% nanocatalyst, which is a ∽10-fold improvement in efficiency compared to heterogeneous catalysts. This research represents a new avenue for the next generation of advanced nanomaterials in catalytic solvent regeneration.

Unraveling the promoting roles of sulfate groups on propane combustion over Pt-SO42−/ZrO2 catalysts

Pt-SO42−/ZrO2 catalysts with different SO42− contents were employed for propane combustion. Addition of SO42− significantly improved the catalytic activity for propane combustion, such as the Pt-5SO42−/ZrO2 catalyst gave the highest turnover frequency (TOF) of 0.56 s−1 at 200 °C, while the pristine Pt/ZrO2 catalyst gave a TOF of only 0.020 s−1. Strong coordination between Pt and SO42− species resulted in drastic suppression of CO adsorption capacity (from 36.8 to 6.0 μmol gcat−1), and increased Pt0 ratio in the spent Pt-SO42−/ZrO2 catalysts. The exposed Pt sites on the Pt/ZrO2 and Pt-SO42−/ZrO2 catalysts show comparable reactivity for C-H activation as evidenced by the methane combustion, and the sulfate species are not helpful in C-H bond cleavage. The enhanced catalytic activities on Pt-SO42−/ZrO2 catalysts for propane combustion are mainly ascribed to the higher reactivity for C-C bond activation promoted by the synergistic catalysis of Pt species with superacid sites. Whereas, such synergy is affected by the amount of SO42− because the excessive SO42− would reduce the exposed Pt sites.

Fabrication of a solid superacid with temperature-regulated silica-isolated biochar nanosheets

This paper reports a new strategy for the structural reconstruction of biomass carbon sulfonic acid (BCSA) to its solid superacid counterpart. In this approach, a cheap layered biomass carbon (BC) source is chemically exfoliated by cetyltrimethyl ammonium bromide and then converted to silica-isolated carbon nanosheets (CNSs) by a series of conversion steps. The state of the silica-isolated CNSs and the stacking density of their nanoparticles are regulated by the dehydration temperature. Only the highly isolated and non-crosslinked CNSs with loose particle stacking structures obtained upon dehydration at 250 °C can be turned into superacid sites (with stronger acidity than that of 100% H2SO4) after sulfonation. This is accompanied by the creation of abundant hierarchical slit pores with high external surface area, mainly driven by the strong hydrogen bonding interactions between the introduced sulfonic acid groups. In typical acid-catalyzed esterification, etherification, and hydrolysis reactions, the newly formed superacid exhibits superior catalytic activity and stability compared to those of common BCSA and commercial Amberlyst-15 catalysts, owing to its good structural stability, highly exposed stable superacidic sites, and abundance of mesoporous/macroporous channels with excellent mass transfer rate. This groundbreaking work not only provides a novel strategy for fabricating bio-based solid superacids, but also overcomes the drawbacks of BCSA, i.e., unsatisfactory structural stability, acidity, and porosity.

CoFe2O4@SiO2-NH-βCD-BF3 as a supramolecular nanocomposite: Synthesis, characterization and catalytic activity

This manuscript describes synthesis of BF3-functionlized β-cylcodextrine grafted magnetic CoFe2O4 nanaoparticles as a hybrid magnetic nano-composite (CoFe2O4@SiO2-NH-βCD-BF3). The CoFe2O4@SiO2-NH-βCD-BF3 was fabricated by grafting of 6-O-toluenesulfonyl cyclodextrin (6-Ts-βCD) to 3-aminopropyl triethoxysilane coated magnetic CoFe2O4@SiO2 nanoparticles followed by combination with BF3. The CoFe2O4@SiO2-NH-βCD-BF3was characterized by FT-IR, TGA, VSM and SEM techniques. The feasibility of using CoFe2O4@SiO2-NH-βCD-BF3 as a magnetically recoverable catalyst was confirmed in the modified-Ritter reaction. The result showed that this novel nano-composite could serve as an efficient nanoreactor bearing super-acidic sites formed by immobilized BF3 and reuse at least for 6 times without loss in activity.

Surface characterization of sulfated zirconia and its catalytic activity for epoxidation reaction of castor oil

The solid acid catalysts SO42−/ZrO2 were prepared by impregnation technique at different calcination temperatures. The surface characterizations were carried out by using scanning electron microscope (SEM), Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), temperature programed desorption of NH3 (NH3-TPD), and N2-BET. The SEM results showed that the size of the SO42−/ZrO2 was not uniform and varied from about 1 to 20 µm. The characteristic peaks in FTIR spectra were essentially the same within the calcination temperature range of 400–700 °C. The XRD results indicated that the transition temperature from amorphous to tetragonal phase was up to 500 °C. The strong acid and superacid sites of the samples could be observed by the NH3-TPD results. The largest BET surface area was 140 m2/g, when the calcination temperature was at 500 °C, and all the pore size distributions belong to mesoporous range. The solid acid SO42−/ZrO2 was used for the epoxidation of castor oil. When the calcination temperature of SO42−/ZrO2 was 600 °C, reaction temperature 45 °C, and reaction time 8 h, the reaction effect was better with an iodine value of 33.0 ± 1.6 g/100 g and an epoxy value of 2.45 ± 0.11 mol/100 g.

Study on the preparation of ordered mesoporous carbon-based catalyst from waste microalgal biomass for the synthesis of biokerosene

Investigation on preparation of novel ordered mesoporous carbon-based catalyst (MCC catalyst) containing super-acid sites from waste microalgal biomass was established. The waste microalgal biomass was partially carbonized at 400 °C for 2 h obtaining biochar; then the obtained biochar was introduced to a sulfonation process using concentrated sulfuric acid. The sulfonation was established at 150 °C for 15 h producing sulfonated biochar. The MCC catalyst was prepared through condensation–evaporation method in an alkaline media containing cetyltrimethylammonium bromide (CTAB) as structure directing agent. The parameters of the condensation including time of evaporating and CTAB content were investigated while fixing temperature at 90 °C during the process. A special hydrothermal treatment was also applied to the preparation of the MCC catalyst in order to expand its mesopores for more convenient with large molecule diffusion. The catalyst activity was well demonstrated by converting linseed oil to biokerosene which could be used as biokerosene—component for blending with aviation fuels. The MCC catalysts were characterized by X-ray diffraction, infrared spectroscopy, energy dispersive X-ray, scanning electron microscopy, transmission electron microscopy, nitrogen adsorption–desorption method and ammonia-temperature programmed desorption techniques. The biokerosene composition was determined by gas chromatography–mass spectroscopy method.

Nanodispersed Suspensions of Zeolite Catalysts for Converting Dimethyl Ether into Olefins

Nanodispersed suspensions that are effective in DME conversion and stable in the reaction zone in a three-phase system (slurry reactor) are obtained from MFI zeolite commercial samples (TsVM, IK-17-1, and CBV) in liquid media via ultrasonic treatment (UST). It is found that the dispersion medium, in which ultrasound affects zeolite commercial sample, has a large influence on particle size in the suspension. UST in the aqueous medium produces zeolite nanoparticles smaller than 50 nm, while larger particles of MFI zeolite samples form in silicone or hydrocarbon oils. Spectral and adsorption data show that when zeolites undergo UST in an aqueous medium, the acid sites are redistributed on the zeolite surface and the specific surface area of the mesopores increases. Preliminary UST in aqueous media of zeolite commercial samples (TsVM, IK-17-1, and CBV) affects the catalytic properties of MFI zeolite nanodispersed suspensions. The selectivity of samples when paraffins and olefins form is largely due to superacid sites consisting of OH groups of hydroxonium ion H3O+.

Surface Characterization of Sulfated Iron Oxide and Its Synthesis of Biodiesel Under Microwave Radiation

AbstractThe solid acid catalysts SO42−/Fe2O3were prepared by impregnation technique, and the preparation conditions were different in calcination temperature, concentration of impregnation solution of H2SO4and impregnation time. The characterization was performed by using Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), Temperature programed desorption of NH3(NH3‒TPD), N2‒BET and microwave absorbing test. As shown by FTIR spectra, the S=O functional group existed in the sample, which was essential for the strong acidity of the SO42‒/MxOytype solid acids. The XRD results indicated that when the calcination temperature exceeded 400℃, iron in SO42‒/Fe2O3transformed from amorphous to crystalline phase. The results from NH3-TPD showed that the prepared sample possessed strong acid and superacid sites. As shown by N2-BET results, the BET surface area of the samples was up to 200m2/g, and their pore size distributions essentially belonged to mesoporous characteristic distribution. The SO42−/Fe2O3solid acid catalysts were used for the transesterification of castor oil under microwave radiation to produce biodiesel. The amounts of FAME in the product were analyzed by high-performance liquid chromatography. The highest yield of product was 65.3 wt.% when the reaction temperature was 65 ℃, alcohol/oil molar ratio was 30/1, catalyst loading was 20 wt.%, the reaction time was 3 h and the power of microwave was 300 w. Furthermore, the reaction results showed that SO42‒/Fe2O3had better catalytic activity under microwave radiation than under conventional heating condition.

Design of novel order mesostructured superacid catalyst from rice husk for the conversion of linseed oil to methyl esters

A novel ordered mesoporous catalyst was prepared from rice husk (MRH catalyst) through condensation–evaporation method in alkaline media. The process used cetyltrimethylammonium bromide (CTAB) as a structure-directing agent (template) and sulfonated biochar obtained from partial rice husk carbonization (SBRH) as precursor. Various parameters such as temperature and CTAB/SBRH mass ratios were investigated to improve the mesoporous structure. The chosen catalyst was based on its degree of order of the mesoporous channels, and its activity was also tested in the methanolysis of linseed oil to methyl esters which was considered as a valuable blending composition for commercial jet fuels. The results showed that the temperature and CTAB/SBRH mass ratio should be of 70 °C and 0.3/1, respectively. The catalyst samples were characterized by many techniques including X-ray diffraction (XRD), infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and ammonia-temperature programmed desorption (NH3-TPD). The methyl ester composition of the as-synthesized biofuel was determined using gas chromatography supported by mass spectroscopy detector (GC–MS). The results of the characterizations showed that the catalyst possessed superacidic sites (NH3-TPD) caused by –SO3H groups (confirmed by FT-IR analysis) and ordered mesoporous structure (XRD). The mesoporous channel distribution was also observed by TEM images. The methanolysis yield reached 93.5% (calculated through GC–MS analysis) at mild conditions with high purity of methyl ester products strongly proving the catalyst activity and selectivity.

Consequence of heterogeneity of active sites for reactivity mechanism of n-butane isomerization over SO42−/ZrO2-Al2O3 catalyst

The relationship between the heterogeneity of active sites and isomerization mechanism of n-butane over alumina-promoted sulfated zirconia (SZA) was elucidated by two series of catalysts with different surface properties. The incomplete removal of coke deposition leads to a decrease in overall activity without the reduction of the rate of isobutane formation. Subjecting the fresh SZA catalyst to the thermal treatment at 650°C causes a striking decrease in activity, resulting from the decrease in the superacidity and oxidizability of the catalyst. While the thermal treatment at 600°C only selectively suppresses the side reactions. It is found that the peaks in NH3-TPD profiles at 500–700°C are caused by a redox reaction between strongly adsorbed ammonia and superacid sites by in situ NH3-TPD-MS measurements. Thus, this peak reflects the strength of superacidity and oxidizability. At the beginning of the reaction, the effective oxidative and protonative activation routes result in the higher concentration of intermediates, which facilitates the “dimerization-isomerization-cracking” reactions. The incomplete removal of coke and the appropriate decrease in the density of sulfate species on the surface selectively promoted the monomolecular pathway.

Ethylbenzene disproportionation and p -xylene selectivity enhancement in xylene isomerization using high crystallinity desilicated H-ZSM-5

Abstract Desilication accompanied with minimum loss of crystallinity effect of a high alumina ZSM-5 zeolite on the isomerization reaction of ethylbenzene/xylene mixtures has been considered. Desilication was assessed through XRF, XRD, FTIR, TEM, nitrogen adsorption/desorption, NH 3 -TPD, 29 Si and 27 Al MAS NMR analytical techniques. Desilication was accompanied with the creation of super acid sites. There exists a limit (Si/Al molar ratio of 9.67) for keeping high crystallinity and obtaining improved catalytic performance. Desilication promotes ethylbenzene conversion by disproportionation and trans-alkylation reactions while the same reactions are limited for the xylene isomers. The p -xylene approach to equilibrium improves by more than 7% at 400 °C and a WHSV of 2 h − 1 for the optimum sample with respect to the parent zeolite. At the same conditions, the optimum sample exhibits the maximum ethylbenzene conversion of 89%, i.e. more than 40% w.r.t. of the parent zeolite. However, the xylene yield decreases only 3%.

Synthesis and study of superacid ZrO2–SiO2–Al2O3 mixed oxide

Strongly acidic ZrO2–SiO2–Al2O3 mixed oxide with different Zr:Si:Al ratios have been synthesized by sol–gel method. It was found that superacid (H0 = −14.52) sites are formed at 12 ≤ Zr4+ ≤ 39, 48 ≤ Si4+ ≤ 72, 3 ≤ Al3+ ≤ 31 at.%. According to the infrared spectra of adsorbed pyridine and acetonitrile-D3, acidic B- and strong L-sites are present on ZrO2–SiO2–Al2O3 surface. Observed high-energy shift of Zr 3d5/2 peak in the X-ray photoelectron spectrum and low-field shift of 29Si nuclear magnetic resonance signal of superacid Zr35Si53Al12 oxide indicate that the electron density transfers from zirconium to silicon atom. The generation of superacidity in ZrO2–SiO2–Al2O3 matrix could be explained by formation of coordinatively unsaturated Zr4+ ions which are strong L-sites. It was shown that superacid ZrO2–SiO2–Al2O3 efficiently catalyzes polymerization of tetrahydrofuran in the presence of acetic anhydride at 40℃ with 68% yield of polytetramethyleneoxide acetate.

Synthesis of tetragonal sulfated zirconia via a novel route for biodiesel production

The sulfated zirconia was prepared by directly impregnating ammonium persulphate on the crystalline zirconia and followed by the calcination temperatures of 300–500°C. The structural properties of the catalysts were characterized by X-ray diffraction (XRD), N2 adsorption-desorption, ammonia temperature programmed desorption (NH3-TPD), Fourier transform infrared spectroscopy (FT-IR) and a scanning electron microscope (SEM) equipped with an energy dispersive spectroscope (EDS). The experiment results demonstrated that the catalysts presented the tetragonal structure of zirconia and high crystallinity. The catalyst calcined at 500°C possessed the highest sulfur content and acidic sites in the catalysts. The catalyst exhibited high catalytic activity in transesterification of soybean oil with methanol. The yield of biodiesel achieved 84.6% because of the preferable super-acid sites on the surface of the catalyst.

Characterization of SO4 2−/TiO2 and its catalytic activity in the epoxidation reaction

The solid acid catalysts SO4 2−/TiO2 were prepared by the impregnation technique under two preparation conditions which were different in calcination temperature and concentration of impregnation solution of H2SO4. The characterization was carried out by using Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), temperature programmed desorption of NH3 (NH3-TPD), N2-BET, X-ray fluorescence and thermal gravity (TG)–differential scanning calorimetry (DSC). The characteristic peaks in the FTIR spectrum were essentially the same within the calcination temperature range of 400–600 °C. The XRD results indicated that the sample could show partial specific peaks of the anatase phase as the calcination temperature was higher than 400 °C. The obvious strong acid and superacid sites of the prepared SO4 2−/TiO2 were conformed by the NH3-TPD results. The BET surface areas of 102–206 m2/g were measured by the N2-BET method, and the pore size distributions were essentially mesoporous. The TG–DSC results showed that SO4 2−/TiO2 would decompose at about 500 °C in the air. The solid acid SO4 2−/TiO2 were used for the epoxidation of castor oil. The lowest iodine value of the product was 52.65/100 g when the reaction temperature was 65 °C, reaction time was 10 h and catalyst loading was 15 wt.%.

Preparation, characterization and thermal stability improvement of mesoporous sulfated zirconia for converting deodorizer distillate to methyl esters

This article reported a new procedure for synthesizing ordered mesoporous sulfated zirconia (m-SZ), an effective oxophosphate process for strengthening thermal stability of the as-synthesized m-SZ catalyst forming mesoporous phosphated sulfated zirconia (m-PSZ). The study also afforded a new reaction routine for synthesizing the m-SZ through condensation method using Zr(SO4)2 solution precursor in the incipient wetness impregnation method. The m-PSZ contained dense surface superacid sites being suitable for methanolysis of almost vegetable oils or animal fats producing methyl ester. The temperature of the condensation process was varied in the range of 70–100 °C, and the time periods were surveyed from 12 to 72 h for well self-assembling the mesoporous structure. The precipitation obtained from the condensations was calcined at 450 °C for 3 h after completely removing of the surface water overnight at 100 °C. The after calcination powder was the m-SZ catalyst. The H3PO4 was used as precursor for oxophosphate process producing the m-PSZ catalyst. The m-PSZ catalyst was applied to the methyl ester synthesis using deodorizer distillate collected from vegetable oil refinery in Vietnam as feedstock. The methanolysis was established at 130 °C for 4 h to obtain the refined methyl esters after passing through a purification process. The refined biodiesel characteristics were determined for its using in diesel engine, and the results showed almost positive values. Some techniques were used in the research such as XRD, TEM, BET, TG–DTA, NH3–TPD and GC–MS.