Insight into solvent-free synthesis of MOR zeolite and its laboratory scale production

Gao, Wan-Yang; Amoo, Cederick Cyril; Javed, Mudassar; Mazonde, Brighton; Lu, Chao; Yang, Renqiang; Tsubaki, Noritatsu

doi:10.1016/j.micromeso.2019.01.041

Cited by 42 publications

(24 citation statements)

References 47 publications

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“…Laboratory works show that the solvent‐free synthesis of zeolites is feasible by milling [14–26] . This method is commonly called mechanochemical.…”

Section: Introductionmentioning

confidence: 99%

“…Laboratory works show that the solvent-free synthesis of zeolites is feasible by milling. [14][15][16][17][18][19][20][21][22][23][24][25][26] This method is commonly called mechanochemical. The process involves the same two basic stages of the conventional synthesis: namely, (i) mixing of the aluminum and silicon precursors with the structuring agent and (ii) crystallization, see Figure 1.…”

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confidence: 99%

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Key Factors During the Milling Stage of the Seed‐assisted and Solvent‐free Synthesis of MFI and Catalytic Behavior in the Alkylation of Phenol with Tert‐butyl Alcohol

et al. 2021

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The so-called mechanochemical method for the synthesis of zeolites reduces the generation of liquid residues and gaseous pollutants as compared to the conventional solvothermal method. Different types of zeolites have been synthesized at the laboratory scale with this method using mostly pestle and mortar. However, such an approach hinders both the systematic comprehension of the effects of the input variables of the milling process and its further scale-up towards the synthesis of the zeolites and their catalytic application. This work investigates the influence of key factors involved in the ball milling stage of the mechanochemical route for the synthesis of MFI done with the assistance of a commercial MFI seed and in the absence of solvents over the most salient physicochemical properties of this type of materials, i.e. the recovery percentage, production cost, morphology, surface area and porosity, crystallinity, acidity of the protonated MFI and catalytic performance. The synthesis of the materials was planned and executed following a full 2 4 factorial experiment whose input variables were the Na2O/SiO2 and H2O/SiO2 molar ratios and the milling time and speed. The effects of both main and interaction factors over key physicochemical properties, and catalytic behavior of the synthesized materials on the alkylation of phenol with tert-butyl alcohol were established within the explored sampling space. Results showed that the Na2O/SiO2 molar ratio plays a key role for the mechanochemical synthesis of MFI, since this variable may direct the synthesis to the preferential production of MOR instead of MFI. On the other hand, it was found that the milling time and speed and their interactions markedly impact the textural properties of MFI. Furthermore, the triple interaction between the input variables affected the concentration of Lewis acid sites of the produced materials. These effects were rationalized by considering that sodium can act as a structure directing agent during the mechanochemical synthesis of MFI and also can promote the incorporation of aluminum to its structure. On the other hand, the milling time and speed are non-linearly correlated to the milling energy required for forming the aluminosilicate precursor that crystallizes during the hydrothermal stage of the process. Overall, all the zeolites synthesized by the mechanochemical route were less crystalline than both the MFI used as seed and an MFI synthesized by solgel. This was associated to the formation of amorphous agglomerates around the zeolitic crystals. Finally, the catalytic behavior of the mechanochemical MFI zeolites in the studied reaction was found to be linearly and positively correlated with both the concentration of BrØnsted of sites and with the density of acid sites. The catalytic tendencies were consistent with the proposal of a stepwise Langmuir-Hinshelwood mechanism for the alkylation of phenol with tert-butyl alcohol.

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“…Laboratory works show that the solvent‐free synthesis of zeolites is feasible by milling [14–26] . This method is commonly called mechanochemical.…”

Section: Introductionmentioning

confidence: 99%

mentioning

confidence: 99%

Key Factors During the Milling Stage of the Seed‐assisted and Solvent‐free Synthesis of MFI and Catalytic Behavior in the Alkylation of Phenol with Tert‐butyl Alcohol

et al. 2021

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“…Gao et al [25] successfully synthesized a high-crystallinity MOR zeolite in laboratoryscale conditions (650 g MOR was produced by 1 L autoclave) through the solvent-free method without an organic template. The specific surface area and pore volume of MOR zeolites synthesized at 473 K for 48 h were 392.1 m 2 •g −1 and 0.314 cm 3 •g −1 , respectively, which are similar to those synthesized by conventional methods (397.9 m 2 •g −1 and 0.093 cm 3 •g −1 ).…”

Section: Solvent-free Synthesis Of Zeolitementioning

confidence: 99%

A Brief Review on Solvent-Free Synthesis of Zeolites

2021

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The traditional hydrothermal method to prepare zeolite will inevitably use a large amount of water as a solvent, which will lead to higher autogenous pressure, low efficiency, and wastewater pollution. The solvent-free method can be used to synthesize various types of zeolites by mechanical mixing, grinding, and heating of solid raw materials, which exhibits the apparent advantages of high yield, low pollution, and high efficiency. This review mainly introduces the development process of solvent-free synthesis, preparation of hierarchical zeolite, morphology control, synthesis mechanism and applications of solvent-free methods. It can be believed that solvent-free methods will become a research focus and have enormous industrial application potential.

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“…Recently, a solvent-free method has been reported for synthesizing zeolites by mixing, grinding, and heating raw solids, which is regarded as a sustainable route. To date, various zeolites, 2 of 10 such as MFI, Beta, FAU, and MOR, have been successfully prepared under this route [18][19][20][21][22]. However, the synthesis of all-silica SOD zeolite has not yet been successful using this sustainable route.…”

Section: Introductionmentioning

confidence: 99%

Sustainable Route for Synthesis of All-Silica SOD Zeolite

Zhai

Bian

et al. 2019

Crystals

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The development of the sustainable synthesis of zeolites has become a very hot topic in recent years. Herein, we report a sustainable route for synthesizing all-silica SOD zeolite under solvent-free conditions. The method of solvent-free synthesis includes mixing, grinding, and heating raw solids. The all-silica SOD zeolite obtained was well characterized by multiple measurement techniques (XRD, SEM, IR, thermogravimetric-differential thermal analysis (TG-DTA), and magic angel spinning nuclear magnetic resonance (MAS NMR)). The crystallization process of all-silica SOD zeolite was also investigated in detail by XRD, SEM, UV-Raman, and MAS NMR techniques. In addition, the effects of the crystallization compositions, including the molar ratios of Na2O/SiO2 and ethylene glycol/SiO2, on the synthesis of the pure all-silica SOD zeolite were investigated at different temperatures.

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Insight into solvent-free synthesis of MOR zeolite and its laboratory scale production

Cited by 42 publications

References 47 publications

Key Factors During the Milling Stage of the Seed‐assisted and Solvent‐free Synthesis of MFI and Catalytic Behavior in the Alkylation of Phenol with Tert‐butyl Alcohol

Key Factors During the Milling Stage of the Seed‐assisted and Solvent‐free Synthesis of MFI and Catalytic Behavior in the Alkylation of Phenol with Tert‐butyl Alcohol

A Brief Review on Solvent-Free Synthesis of Zeolites

Sustainable Route for Synthesis of All-Silica SOD Zeolite

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