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Liquid-phase hydrogenation of carbon tetrachloride catalyzed by three-dimensional graphene-supported palladium catalyst

  • Zhuoyi Xie and Jianwei Guo EMAIL logo
Published/Copyright: August 5, 2022
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Green Processing and Synthesis
From the journal Green Processing and Synthesis Volume 11 Issue 1

Abstract

In this article, a three-dimensional graphene (3DGN)-supported palladium metal catalyst was prepared by the impregnation method with noble metal palladium as the active component, aiming to synthesize a catalyst with high activity and high selectivity. Its catalytic performance in liquid-phase hydrochlorination of carbon tetrachloride (TTCM) was investigated. The influences of different Pd loadings, reduction temperatures, and reaction temperatures on the catalytic hydrogenation reaction were studied. The purpose is to explore the best operating conditions for the preparation of chloroform. The results show that the 3DGN-supported palladium catalyst exhibits excellent catalytic performance and high selectivity to chloroform in the hydrogenation of TTCM. When the Pd loading was 1.0 wt%, the reduction temperature was 773 K, and the hydrochlorination reaction temperature was 398 K, the conversion of TTCM was as high as 98.12%, and the selectivity of chloroform was 85.23%. The main by-product is dichloromethane. The selectivity of chloroform is affected by the increasing temperature but remains above 80%.

Keywords: carbon tetrachloride; hydrochlorination; palladium/three-dimensional graphene catalyst; selectivity

1 Introduction

Carbon tetrachloride (TTCM) has been widely used as a fire extinguishing agent, a chlorinating agent for organic substances, and an organic solvent, but its production is now restricted due to its toxicity and destruction of the ozone layer. After the Montreal Protocol (1987), the Cooperation further reduced the manufacture and use of chlorofluorocarbon and the production market for TTCM gradually declined. It has been listed among the compounds banned from emission after several years at the London Conference in 1990. TTCM is a by-product of many industrial chlorination processes, so the green conversion of TTCM is essential. Catalytic hydrochlorination has become one of the most promising green conversion methods compared to other methods. Delannoy et al. studied the hydrochlorination of TTCM on Group VI metal carbides (WC, W2C, and Mo2C). These carbides were prepared by temperature-programmed carburizing of WO3 and MoO3 in 10–20% CH4/H2 mixtures. Mo2C and W2C were rapidly deactivated with time, independent of temperature, whereas WC showed good stability at 393 K [1]. Lu et al. obtained the lower surface activation energy of Pt(111) by studying its surface adsorption and hydrogenation. It shows that a platinum catalyst has high catalytic activity for the TTCM hydrogenation reaction [2]. Bonarowska et al. found that alumina-supported platinum’s catalytic activity is strongly dependent on metal dispersion. At 343–363 K, the catalytic activity of Pt/Al2O3 in TTCM hydrochlorination was inversely proportional to the dispersion of platinum [3]. A report on multimetallic catalysts found that the activated carbon-supported Pd–Au catalyst exhibited much better performance than the monometallic Pd sample in the hydrochlorination of TTCM. Pd–Au mixing was critical to obtain this synergistic effect [4]. The synergistic effect of the alloy will effectively improve the performance of the catalyst. Similarly, Karpinski et al. studied the hydrogenation of TTCM on SiO2-supported Pd–Au alloy, and the reasonably mixed Pd–Au particles showed better catalytic performance in about 60 h. At the same time, the single metal palladium and palladium-rich catalysts would be inactivated rapidly [5]. Bae et al. studied tin’s effect on Pt–Sn/γ-Al2O3 in TTCM hydrochlorination reaction [6]. It is concluded that the Pt–Sn/γ-Al2O3 catalyst with an appropriate amount of tin exhibits enhanced catalytic stability and selectivity to CHCl3 in the hydrochlorination of TTCM [6]. Although the catalysts studied above have a certain catalytic effect, their selectivity to chloroform is still low. The catalyst synthesis process was complicated because the catalyst was easily deactivated and had poor stability. Therefore, the preparation of catalysts with high activity and selectivity is of great significance for industrial applications.

Metallic palladium is a catalyst for hydrogen activation to form free atomic hydrogen, which is a reducing agent for dechlorination and hydrogenation of organic halogens [7–9]. Pd-based catalysts exhibit high catalytic activity and selectivity at lower reaction temperatures. Three-dimensional graphene (3DGN) as a carrier can provide a larger specific surface area, improve the dispersibility of metal particles, and reduce the agglomeration of metal particles in the hydrochlorination reaction. Notably, the conjugated structure of 3DGN can provide a better ability to adsorb molecules and higher electron mobility on the surface. It is conducive to the transfer of electrons on the carrier surface, thereby improving the catalytic activity of metals [10]. Both refer to three-dimensional graphene and palladium metal.

In order to improve the selectivity of chloroform and optimize the reaction process, this article combines the excellent properties of 3D graphene and palladium metal. A series of catalysts with different Pd loadings were prepared using the self-made 3D graphene as the carrier. The catalytic performance of 3DGN-loaded palladium metal catalysts (Pd/3DGNs) in the TTCM hydrogenation reaction was investigated using intermittent reactions.

2 Materials and methods

2.1 Reagents and materials

Expanded graphite (purity ≥99.7%) was purchased from Jiangsu Xianfeng Nanomaterials Technology Co., Ltd. Sodium nitrate (NaNO3, 99.5%), H2SO4 (98%), potassium permanganate (KMnO4, 98.0%), H2O2 (30%), HCl (5%), palladium chloride (PdCl2), TTCM (CCl4, 99%), and n-hexane (98%) were purchased from Guangzhou Ruoyang Huabo Instrument Co., Ltd. Hydrogen (high purity hydrogen, 99.999%) was purchased from Guangzhou Danoutong Trading Co., Ltd.

2.2 Preparation of 3DGN

Graphene oxide (GO) was prepared using expanded graphite as raw material by the classical modified Hummers method [11]. The obtained GO is put into the stainless-steel hydrothermal reactor lined with 50 mL polytetrafluoroethylene. It was placed in a muffle furnace and heated to 180°C for 24 h. After cooling to room temperature, the samples were soaked in deionized water for 12 h. The samples were taken out and then freeze-dried in a freeze dryer (model SR-A10N-50) at −50°C for 48 h to obtain 3DGNs.

2.3 Preparation of 3DGN-supported palladium metal catalyst

The catalyst precursors with different Pd mass fractions (0.2, 0.3, 0.5, 1.0, and 1.5 wt%) were obtained after 12 h impregnation of 3DGN carriers using different concentrations of aqueous H2PdCl4 solutions (prepared from 0.02, 0.03, 0.05, 0.10, and 0.15 g anhydrous PdCl2 and concentrated HCl). The catalyst precursors with different Pd mass fractions were obtained. After drying at 393 K for 48 h, the Pd catalyst precursor was placed in a tube furnace. The samples were reduced at 523, 573, 773, and 973 K for 6 h under an H2 (5%)/Ar (95%) mixed gas flow rate of 20 mL·min−1. After the reaction was completed, it was cooled to room temperature, taken out, and sealed for later use. The catalysts were then labeled as 0.2, 0.3, 0.5, 1.0, and 1.5 Pd/3DGNs, respectively.

2.4 Characterization of catalyst

The molecular structures of GO, 3DGNs, and catalysts were analyzed by UV laser Raman spectroscopy (LabRAM hr800). X-ray diffraction (XRD) patterns were collected on an X-ray Diffractometer model (D8 ADVANCE) to analyze the crystalline phases of GO, 3DGNs, and catalysts. The morphology and microstructure of GO and 3DGNs were analyzed by field emission scanning electron microscopy (JSM-7001F, SEM). The porous structure of 3DGNs was characterized by specific surface area and micropore physical adsorption analyzer (ASAP2020). High-resolution transmission electron microscopy (TEM) was used to determine the structure of 3DGNs using the model HT7700. X-ray photoelectron spectroscopy (XPS; ESCALAB 250Xi) was used to determine the surface composition of the catalyst and the compound state of the elements.

2.5 Evaluation of catalyst

The catalyst’s performance was evaluated by the hydrogenation and dechlorination of TTCM. The reaction was carried out in a fully automated parallel reactor produced in France (TOP HPHT 200). The equipment was installed after adding 50 mL of CCl4, 6 g of Pd/3DGN catalyst, and 50 mL of n-hexane solvent to the autoclave in sequence. Before the reaction, the entire system was replaced with 1 MPa nitrogen five times and then replaced with 1 MPa hydrogen five times. After passing hydrogen to the pressure of 3 MPa, the temperature was raised to the set reaction temperature. The reaction products were analyzed quantitatively and qualitatively by gas chromatography (Agilent 7820 GC) on a P/N 19091J-413, HP-5 capillary column of 30 m × 320 μm × 0.25 μm.

3 Results and discussion

3.1 Characterization of catalyst

In order to study the morphology and surface microstructure of GO, 3DGNs, and catalysts, they were characterized by SEM and TEM, and the results are shown in Figure 1. Figure 1a shows the SEM image of GO. It can be seen that the appearance of GO is a monolithic structure with a wrinkled surface. Figure 1b and c shows the 3DGNs after high-temperature hydrothermal reduction. Its interior presents a highly cross-linked network structure with many holes, which provides a prerequisite for the high dispersion of metal atoms in the active center of the catalyst. The irregular internal structure of 3DGNs can be seen from the TEM image of 3DGNs in Figure 1d. The darker color parts exhibit a high degree of aggregation of nanostructures. Figure 1e and f shows the TEM images of the 1.0 Pd/3DGN catalyst at different magnifications, respectively. It can be seen that the palladium metal is evenly distributed along the folds and edges of the carrier. This indicates a strong interaction between palladium metal and 3DGN support [12–15]. In order to further explore the specific surface area of the 3DGN support, it was characterized by Brunauer, Emmett and Teller (BET) and compared with other catalyst supports, as shown in Table 1. It can be seen that the specific surface area of the self-made 3DGN carrier is 358 m2·g−1, which is higher than that of the other carriers in the table. This enables the metal crystals to attach and disperse on the surface and mass transfer during the reaction, providing more active sites. Graphene as a catalytic carrier can provide a larger specific surface area and excellent morphological stability and effectively improve dispersibility [16,17]. At the same time, the dispersibility and stability of palladium metal on the surface of the carrier are effectively improved.

Figure 1 SEM and TEM results: (a) SEM image of GO, (b and c) SEM images of 3DGNs, (d) TEM image of 3DGNs, (e and f) TEM images of 1.0 Pd/3DGN catalyst.
Figure 1

SEM and TEM results: (a) SEM image of GO, (b and c) SEM images of 3DGNs, (d) TEM image of 3DGNs, (e and f) TEM images of 1.0 Pd/3DGN catalyst.

Table 1

Comparison of specific surface areas of different catalyst supports

Catalyst support S BET (m2·g−1) Average pore diameter (nm) Reference
3DGNs 358 28.8 —
Al2O3 180 — [33]
AlF3 72 — [34]
MgO 152 10.5 [35]

To reveal the extent of reduction of GO, 3DGNs, and 1.0 Pd/3DGN catalysts, they were characterized by Raman spectroscopy. The results are shown in Figure 2. It can be seen from Figure 2 that all samples have two peak bands at 1,350 and 1,590 cm−1. They are called D-peak and G-peak, respectively. The D peak is the defect peak of carbon lattice sp3 hybridization, and the G peak is the carbon–carbon double bond peak [18,19]. The D/G band intensity ratio reflects the degree of graphitization [20,21]. The smaller the I D/I G ratio, the higher the degree of graphitization and reduction. From the data obtained in the figure, it can be calculated that the corresponding I D/I G of GO, 3DGNs, and 1.0 Pd/3DGN catalysts are 1.33, 1.21, and 1.02, respectively. It shows that compared with GO and 3DGNs, the degree of graphitization of 1.0 Pd/3DGN catalyst is increased, and the reduction effect is better. In addition, a peak at 2,700 cm−1 appeared on the spectrum of the 1.0 Pd/3DGN catalyst. This is the 2D band of graphene, and the appearance of the 2D band proves the better quality and properties of graphene [22,23].

Figure 2 Raman spectra of GO, 3DGNs, and 1.0 Pd/3DGN catalysts.
Figure 2

Raman spectra of GO, 3DGNs, and 1.0 Pd/3DGN catalysts.

In order to conduct phase analysis of GO, 3DGNs, and 1.0 Pd/3DGN catalysts, they were examined by XRD with loadings of 0.2, 0.3, 0.5, 1.0, and 1.5 wt%. The result is shown in Figure 3. It can be seen that the diffraction peak of GO appears at 2θ = 10.3°. According to Bragg’s law (Eq. 1), the distance between the GO layers is calculated to be 0.86 nm [24]. In addition, at 26.4°, both the 3DGNs and the reduced catalyst have this characteristic peak. The chemically reduced graphene sheets are re-stacked to form a regular and periodic graphitic-like layered structure. The sp2 hybrid graphene network was re-established in the reduction. These phenomena can be confirmed from the SEM images. This characteristic peak can be found in the XRD patterns of the Pd/3DGN catalyst, which proves that the high-temperature reduction does not destroy the three-dimensional structure of the support. The characteristic peaks of palladium metal crystals appear on the (111), (200), and (220) planes. From the XRD pattern of the Pd/3DGN catalyst, it can be seen that the metal crystal peaks are prominent, and more crystals are attached to the surface of the material. When the loading of palladium metal is within 1.0 wt%, relatively broad diffraction peaks are obtained, indicating that the metal crystal size is minimal. Due to the small percentage and particle size, the diffraction signal of metallic palladium cannot be detected [25]. It shows that the metal palladium crystals form a monolayer or sub-monolayer dispersion on the 3DGN support. This dispersed state is a thermodynamically stable state, which will be beneficial to improving the activity and stability of the catalyst [26]. When the loading of palladium metal is 1.5 wt%, the characteristic peaks of metal crystals are more prominent due to the agglomeration of metal palladium. This is probably one of the reasons why the catalyst activity of the supported amount is not very high.

(1) 2 d sin θ = n λ

Figure 3 XRD spectra of GO, 3DGNs, and 0.2, 0.3, 0.5, 1.0, and 1.5 wt% Pd catalysts.
Figure 3

XRD spectra of GO, 3DGNs, and 0.2, 0.3, 0.5, 1.0, and 1.5 wt% Pd catalysts.

3.2 Evaluation of catalyst

3.2.1 Effects of Pd loading and reaction temperature on the reaction performance of Pd/3DGN catalyst

The catalyst’s performance was investigated by changing the loading of palladium metal and the reaction temperature. The results are shown in Table 2. The metal loading shows that the conversion rate of TTCM and the selectivity of chloroform of 1.0 wt% Pd catalyst are high, and the selectivity of chloroform is 85.23%. It can be seen that the high loading of Pd has a favorable effect on the reaction rate. However, when the loading of Pd was set at 1.5 wt%, the conversion rate of TTCM did not improve much. This is because of the agglomeration of palladium metal, which was confirmed by the XRD results. Since palladium is a precious metal, its loading should not be too large. Otherwise, the cost of the catalyst is too high, and when the loading is too large, a part of the active components agglomerates or stays in the deep pores of the support. The hydrogenation activity of the catalyst will be reduced, so the loading amount of 1.0 wt% is the most suitable. The effect of temperature on TTCM conversion was investigated at 358, 378, 398, and 418 K using a 1.0 wt% Pd/3DGN catalyst. The increase in reaction temperature results in the enrichment of by-products. The selectivity of dichloromethane was as high as 14.98% at the reaction temperature of 418 K. From the point of view of reaction time and reaction conditions, 398 K is the most suitable reaction temperature, with low cost and high chloroform selectivity. It can be seen from Table 2 that the conversion rate of TTCM in most catalytic systems can reach 90–100%, but the selectivity to chloroform is slightly different. Among them, the selectivity of chloroform in the Ir/SiO2 catalyst reaction system is the highest at 92.43%. However, considering the cost, this method is not suitable for industrialization. The chloroform selectivity of the 3DGN supported Pd/3DGN catalyst prepared in this article is 85.23% in this reaction system. This catalyst has potential industrial application value.

Table 2

Comparison of activity and selectivity of different catalytic systems for hydrogenation of carbon tetrachloride

Catalyst Reaction temperature (K) CCl4 conversion rate (%) CHCl3 selectivity (%) CH2Cl2 selectivity (%)
0.2 Pd/3DGNs 398 50.32 80.16 —
0.3 Pd/3DGNs 398 55.15 80.57 —
0.5 Pd/3DGNs 398 70.63 80.69 —
1.5 Pd/3DGNs 398 98.08 83.01 —
1.0 Pd/3DGNs 358 80.36 81.32 9.12
1.0 Pd/3DGNs 378 85.49 80.79 10.56
1.0 Pd/3DGNs 398 98.12 85.23 12.69
1.0 Pd/3DGNs 418 98.09 82.45 14.98
Pt/Al2O3 [36] — 97.6 69.0 —
Pd/MgO–MgF2 [35] — 100 <62.7 —
Ir/SiO2 [37] — 92.50 92.43 —

3.2.2 Effect of reduction temperature on the reaction performance of Pd/3DGN catalyst

In order to study the effect of reduction temperature on the reaction performance of the catalyst, the valence state of the metal on the catalyst was characterized by XPS. The results are shown in Figure 4. It can be seen that Pd n+ peaks appear at 338 and 343 eV, and Pd0 peaks appear at 335.8 and 337.7 eV on Pd/3DGNs [27]. There are two reasons for the appearance of the Pd n+ peak after the catalyst is reduced at a high temperature to obtain Pd0. First, the catalyst is not fully reduced, as there is still a tiny amount of Pd2+. Second, due to the fact that the catalyst is exposed to air after reduction, an oxide film is formed on the surface of Pd0. The reduction temperature rises from 523 to 973 K. The content of palladium metal increases continuously. The higher the reduction temperature, the more palladium metal Pd0 is obtained. It can be seen from Table 3 that the selectivity of chloroform varies with the surface atomic ratio of Pd0/Pd n+. TTCM showed lower chloroform selectivity in catalysts with a Pd0/Pd n+ ratio higher or lower than 1. When the Pd0/Pd n+ atomic ratio is close to 1, the chloroform selectivity is higher. The Pd/3DGN catalyst at the reduction temperature of 773 K has the best selectivity of chloroform.

Figure 4 XPS spectra: reduction of 1.0 Pd/3DGNs at (a) 973 K, (b) 773 K, (c) 573 K, and (d) 523 K.
Figure 4

XPS spectra: reduction of 1.0 Pd/3DGNs at (a) 973 K, (b) 773 K, (c) 573 K, and (d) 523 K.

Table 3

Effect of the reduction temperature on the catalytic performance

Reduction temperature (K) Pd0/Pd n+ S TCM (%)
523 0.01 80.65
573 0.35 82.96
773 0.98 85.23
973 2.96 81.63

Note: catalyst, 1.0 Pd/3DGNs; reaction temperature, 398 K; and hydrogen pressure, 3 MPa. S TCM indicates chloroform selectivity.

As mentioned before, chloroform was the main product in all reactions, and its reactivity was very low (Table 2). The sum of the selectivities for chloroform and dichloromethane was approximately constant throughout the reaction. This experimental result confirms that dichloromethane was converted from chloroform. Therefore, the TTCM reaction is a continuous dechlorination reaction.

The first step of the reaction is the adsorption of TTCM and hydrogen on the catalyst surface. The results given in Table 3 show that the reduction temperature changes the valence state of the metal Pd on the catalyst surface. The reduction temperature affects the distribution of Pd0 and Pd n+, thereby affecting the catalytic activity of the catalyst. When the reduction temperature is 523 K, the Pd0/Pd n+ ratio is 0.01, and the selectivity of chloroform is only 80.65%. When the reduction temperature reached 773 K, the ratio of Pd0/Pd n+ increased to 0.98, and the selectivity of chloroform increased to 85.23%. When the reduction temperature increased to 973 K, the ratio of Pd0/Pd n+ reached 2.96, but the selectivity of chloroform decreased to 81.63%. The above discussion shows that Pd0 and Pd n+ are necessary for the catalytic dechlorination reaction. The active centers of Pd/3DGN catalysts in this reaction are formed by the combination of adjacent metal and electron-deficient palladium species [Pd0 + Pd n+], which can be confirmed in many kinds of literature [28,29].

(2) 2 Pd 0 + H 2 → 2 H–Pd 0

(3) Pd n + + Cl ⋯ CCl 3 → [ Cl - Pd ] n + + • CCl 3

(4) H - Pd 0 + • CCl 3 → CHCl 3 + Pd 0

(5) [ Cl - Pd ] n + + H - Pd 0 → HCl + Pd n + + Pd 0

As shown in Eqs. 2 and 3, Pd0 adsorbs H2 and dissociates into adatom H–Pd0, while TTCM adsorbs on a single Pd n+ site. As shown in Eqs. 4 and 5, the adsorbed TTCM is hydrogenated to form chloroform. Cl− is rapidly and gradually replaced by hydrogen atoms to form HCl. This synergistic mechanism has also been reported in other literature [30]. A truly continuous process in which the adsorbed phases on the same active center occur via a “rake” mechanism is considered a synergistic mechanism [31]. Therefore, the high selectivity of chloroform can be understood as the high selectivity of Pd n+ to chloroform radicals.

(6) Pd n + + Cl ⋯ CHCl 2 → [ Cl - Pd ] n + + • CHCl 2

(7) H - Pd 0 + • CHCl 2 → CH 2 Cl 2 + Pd 0

The second step of the reaction is the adsorption of chloroform and hydrogen on the catalyst surface. The chloroform generated by the first-step reaction regenerates the activation center and reacts with H–Pd0 to form dichloromethane, as shown in Eqs. 6 and 7. But in the reaction from chloroform to dichloromethane, the energy required to remove one chlorine atom increased from 285.9 to 349.0 kJ·mol−1 [32]. Therefore, the difficulty of generating dichloromethane increases. It is proved by experiments that the selectivity of dichloromethane increases with the increase in reaction temperature. The reason is that the temperature increase promotes the reaction (Eq. 6). Therefore, the concentration of dichloromethane increases. It can be seen that the formation of dichloromethane is due to the adsorption and dissociation of a small part of chloroform on the Pd/3DGN catalyst. Therefore, in order to improve the selectivity of chloroform, the reaction temperature should be in a moderate range.

4 Conclusion

In this study, a 3DGN catalyst carrier was successfully synthesized. The support has a larger specific surface area and porous structure to provide more active sites with a higher degree of graphitization. The palladium metal is more fully and stably attached to the surface of the carrier. The TEM and SEM results show that 3DGNs as catalyst carriers can significantly improve the dispersion of metal particles. The results showed that the selectivity of TTCM to chloroform was higher at a Pd loading of 1.0 wt%, a reduction temperature of 773 K, and a hydrochlorination reaction temperature of 398 K. The main by-product of the reaction is methylene chloride. The higher the reaction temperature, the higher the dichloromethane content as a by-product and the lower the selectivity of chloroform, but it always remained above 80%.

  1. Funding information: The authors state no funding involved.

  2. Author contributions: Jianwei Guo: writing – review and editing, supervision, resources, methodology, project administration; Zhuoyi Xie: writing – original draft, software, data curation, investigation.

  3. Conflict of interest: The authors state no conflict of interest.

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Received: 2022-03-30
Revised: 2022-05-25
Accepted: 2022-05-30
Published Online: 2022-08-05

© 2022 Zhuoyi Xie and Jianwei Guo, published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  3. Black pepper (Piper nigrum) fruit-based gold nanoparticles (BP-AuNPs): Synthesis, characterization, biological activities, and catalytic applications – A green approach
  4. Protective role of foliar application of green-synthesized silver nanoparticles against wheat stripe rust disease caused by Puccinia striiformis
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  6. Efficient degradation of methyl orange and methylene blue in aqueous solution using a novel Fenton-like catalyst of CuCo-ZIFs
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  8. Efficient pilot-scale synthesis of the key cefonicid intermediate at room temperature
  9. Synthesis and characterization of noble metal/metal oxide nanoparticles and their potential antidiabetic effect on biochemical parameters and wound healing
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https://doi.org/10.1515/gps-2022-0066
Keywords for this article
carbon tetrachloride; hydrochlorination; palladium/three-dimensional graphene catalyst; selectivity
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Kinetic study on the reaction between Incoloy 825 alloy and low-fluoride slag for electroslag remelting
  3. Black pepper (Piper nigrum) fruit-based gold nanoparticles (BP-AuNPs): Synthesis, characterization, biological activities, and catalytic applications – A green approach
  4. Protective role of foliar application of green-synthesized silver nanoparticles against wheat stripe rust disease caused by Puccinia striiformis
  5. Effects of nitrogen and phosphorus on Microcystis aeruginosa growth and microcystin production
  6. Efficient degradation of methyl orange and methylene blue in aqueous solution using a novel Fenton-like catalyst of CuCo-ZIFs
  7. Synthesis of biological base oils by a green process
  8. Efficient pilot-scale synthesis of the key cefonicid intermediate at room temperature
  9. Synthesis and characterization of noble metal/metal oxide nanoparticles and their potential antidiabetic effect on biochemical parameters and wound healing
  10. Regioselectivity in the reaction of 5-amino-3-anilino-1H-pyrazole-4-carbonitrile with cinnamonitriles and enaminones: Synthesis of functionally substituted pyrazolo[1,5-a]pyrimidine derivatives
  11. A numerical study on the in-nozzle cavitating flow and near-field atomization of cylindrical, V-type, and Y-type intersecting hole nozzles using the LES-VOF method
  12. Synthesis and characterization of Ce-doped TiO2 nanoparticles and their enhanced anticancer activity in Y79 retinoblastoma cancer cells
  13. Aspects of the physiochemical properties of SARS-CoV-2 to prevent S-protein receptor binding using Arabic gum
  14. Sonochemical synthesis of protein microcapsules loaded with traditional Chinese herb extracts
  15. MW-assisted hydrolysis of phosphinates in the presence of PTSA as the catalyst, and as a MW absorber
  16. Fabrication of silicotungstic acid immobilized on Ce-based MOF and embedded in Zr-based MOF matrix for green fatty acid esterification
  17. Superior photocatalytic degradation performance for gaseous toluene by 3D g-C3N4-reduced graphene oxide gels
  18. Catalytic performance of Na/Ca-based fluxes for coal char gasification
  19. Slow pyrolysis of waste navel orange peels with metal oxide catalysts to produce high-grade bio-oil
  20. Development and butyrylcholinesterase/monoamine oxidase inhibition potential of PVA-Berberis lycium nanofibers
  21. Influence of biosynthesized silver nanoparticles using red alga Corallina elongata on broiler chicks’ performance
  22. Green synthesis, characterization, cytotoxicity, and antimicrobial activity of iron oxide nanoparticles using Nigella sativa seed extract
  23. Vitamin supplements enhance Spirulina platensis biomass and phytochemical contents
  24. Malachite green dye removal using ceramsite-supported nanoscale zero-valent iron in a fixed-bed reactor
  25. Green synthesis of manganese-doped superparamagnetic iron oxide nanoparticles for the effective removal of Pb(ii) from aqueous solutions
  26. Desalination technology for energy-efficient and low-cost water production: A bibliometric analysis
  27. Biological fabrication of zinc oxide nanoparticles from Nepeta cataria potentially produces apoptosis through inhibition of proliferative markers in ovarian cancer
  28. Effect of stabilizers on Mn ZnSe quantum dots synthesized by using green method
  29. Calcium oxide addition and ultrasonic pretreatment-assisted hydrothermal carbonization of granatum for adsorption of lead
  30. Fe3O4@SiO2 nanoflakes synthesized using biogenic silica from Salacca zalacca leaf ash and the mechanistic insight into adsorption and photocatalytic wet peroxidation of dye
  31. Facile route of synthesis of silver nanoparticles templated bacterial cellulose, characterization, and its antibacterial application
  32. Synergistic in vitro anticancer actions of decorated selenium nanoparticles with fucoidan/Reishi extract against colorectal adenocarcinoma cells
  33. Preparation of the micro-size flake silver powders by using a micro-jet reactor
  34. Effect of direct coal liquefaction residue on the properties of fine blue-coke-based activated coke
  35. Integration of microwave co-torrefaction with helical lift for pellet fuel production
  36. Cytotoxicity of green-synthesized silver nanoparticles by Adansonia digitata fruit extract against HTC116 and SW480 human colon cancer cell lines
  37. Optimization of biochar preparation process and carbon sequestration effect of pruned wolfberry branches
  38. Anticancer potential of biogenic silver nanoparticles using the stem extract of Commiphora gileadensis against human colon cancer cells
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  40. First report of biocellulose production by an indigenous yeast, Pichia kudriavzevii USM-YBP2
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  45. Anti-colon cancer activities of green-synthesized Moringa oleifera–AgNPs against human colon cancer cells
  46. Phosphorus removal from aqueous solution by adsorption using wetland-based biochar: Batch experiment
  47. A low-cost and eco-friendly fabrication of an MCDI-utilized PVA/SSA/GA cation exchange membrane
  48. Synthesis, microstructure, and phase transition characteristics of Gd/Nd-doped nano VO2 powders
  49. Biomediated synthesis of ZnO quantum dots decorated attapulgite nanocomposites for improved antibacterial properties
  50. Preparation of metal–organic frameworks by microwave-assisted ball milling for the removal of CR from wastewater
  51. A green approach in the biological base oil process
  52. A cost-effective and eco-friendly biosorption technology for complete removal of nickel ions from an aqueous solution: Optimization of process variables
  53. Protective role of Spirulina platensis liquid extract against salinity stress effects on Triticum aestivum L.
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  55. Effectiveness of different accelerated green synthesis methods in zinc oxide nanoparticles using red pepper extract: Synthesis and characterization
  56. Blueprinting morpho-anatomical episodes via green silver nanoparticles foliation
  57. A numerical study on the effects of bowl and nozzle geometry on performances of an engine fueled with diesel or bio-diesel fuels
  58. Liquid-phase hydrogenation of carbon tetrachloride catalyzed by three-dimensional graphene-supported palladium catalyst
  59. The catalytic performance of acid-modified Hβ molecular sieves for environmentally friendly acylation of 2-methylnaphthalene
  60. A study of the precipitation of cerium oxide synthesized from rare earth sources used as the catalyst for biodiesel production
  61. Larvicidal potential of Cipadessa baccifera leaf extract-synthesized zinc nanoparticles against three major mosquito vectors
  62. Fabrication of green nanoinsecticides from agri-waste of corn silk and its larvicidal and antibiofilm properties
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  64. Study on the functionalization of activated carbon and the effect of binder toward capacitive deionization application
  65. Co-chlorination of low-density polyethylene in paraffin: An intensified green process alternative to conventional solvent-based chlorination
  66. Antioxidant and photocatalytic properties of zinc oxide nanoparticles phyto-fabricated using the aqueous leaf extract of Sida acuta
  67. Recovery of cobalt from spent lithium-ion battery cathode materials by using choline chloride-based deep eutectic solvent
  68. Synthesis of insoluble sulfur and development of green technology based on Aspen Plus simulation
  69. Photodegradation of methyl orange under solar irradiation on Fe-doped ZnO nanoparticles synthesized using wild olive leaf extract
  70. A facile and universal method to purify silica from natural sand
  71. Green synthesis of silver nanoparticles using Atalantia monophylla: A potential eco-friendly agent for controlling blood-sucking vectors
  72. Endophytic bacterial strain, Brevibacillus brevis-mediated green synthesis of copper oxide nanoparticles, characterization, antifungal, in vitro cytotoxicity, and larvicidal activity
  73. Off-gas detection and treatment for green air-plasma process
  74. Ultrasonic-assisted food grade nanoemulsion preparation from clove bud essential oil and evaluation of its antioxidant and antibacterial activity
  75. Construction of mercury ion fluorescence system in water samples and art materials and fluorescence detection method for rhodamine B derivatives
  76. Hydroxyapatite/TPU/PLA nanocomposites: Morphological, dynamic-mechanical, and thermal study
  77. Potential of anaerobic co-digestion of acidic fruit processing waste and waste-activated sludge for biogas production
  78. Synthesis and characterization of ZnO–TiO2–chitosan–escin metallic nanocomposites: Evaluation of their antimicrobial and anticancer activities
  79. Nitrogen removal characteristics of wet–dry alternative constructed wetlands
  80. Structural properties and reactivity variations of wheat straw char catalysts in volatile reforming
  81. Microfluidic plasma: Novel process intensification strategy
  82. Antibacterial and photocatalytic activity of visible-light-induced synthesized gold nanoparticles by using Lantana camara flower extract
  83. Antimicrobial edible materials via nano-modifications for food safety applications
  84. Biosynthesis of nano-curcumin/nano-selenium composite and their potentialities as bactericides against fish-borne pathogens
  85. Exploring the effect of silver nanoparticles on gene expression in colon cancer cell line HCT116
  86. Chemical synthesis, characterization, and dose optimization of chitosan-based nanoparticles of clodinofop propargyl and fenoxaprop-p-ethyl for management of Phalaris minor (little seed canary grass): First report
  87. Double [3 + 2] cycloadditions for diastereoselective synthesis of spirooxindole pyrrolizidines
  88. Green synthesis of silver nanoparticles and their antibacterial activities
  89. Review Articles
  90. A comprehensive review on green synthesis of titanium dioxide nanoparticles and their diverse biomedical applications
  91. Applications of polyaniline-impregnated silica gel-based nanocomposites in wastewater treatment as an efficient adsorbent of some important organic dyes
  92. Green synthesis of nano-propolis and nanoparticles (Se and Ag) from ethanolic extract of propolis, their biochemical characterization: A review
  93. Advances in novel activation methods to perform green organic synthesis using recyclable heteropolyacid catalysis
  94. Limitations of nanomaterials insights in green chemistry sustainable route: Review on novel applications
  95. Special Issue: Use of magnetic resonance in profiling bioactive metabolites and its applications (Guest Editors: Plalanoivel Velmurugan et al.)
  96. Stomach-affecting intestinal parasites as a precursor model of Pheretima posthuma treated with anthelmintic drug from Dodonaea viscosa Linn.
  97. Anti-asthmatic activity of Saudi herbal composites from plants Bacopa monnieri and Euphorbia hirta on Guinea pigs
  98. Embedding green synthesized zinc oxide nanoparticles in cotton fabrics and assessment of their antibacterial wound healing and cytotoxic properties: An eco-friendly approach
  99. Synthetic pathway of 2-fluoro-N,N-diphenylbenzamide with opto-electrical properties: NMR, FT-IR, UV-Vis spectroscopic, and DFT computational studies of the first-order nonlinear optical organic single crystal
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