scholarly journals Fast Production of Cellulose Nanocrystals by Hydrolytic-Oxidative Microwave-Assisted Treatment

Polymers ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 68 ◽  
Author(s):  
Luana Amoroso ◽  
Giuseppe Muratore ◽  
Marco Aldo Ortenzi ◽  
Stefano Gazzotti ◽  
Sara Limbo ◽  
...  

In contrast to conventional approaches, which are considered to be energy- and time-intensive, expensive, and not green, herein, we report an alternative microwave-assisted ammonium persulfate (APS) method for cellulose nanocrystals (CNCs) production, under pressurized conditions in a closed reaction system. The aim was to optimize the hydrolytic-oxidative patented procedure (US 8,900,706), replacing the conventional heating with a faster process that would allow the industrial scale production of the nanomaterial and make it more appealing to a green economy. A microwave-assisted process was performed according to different time–temperature programs, varying the ramp (from 5 to 40 min) and the hold heating time (from 60 to 90 min), at a fixed reagent concentration and weight ratio of the raw material/APS solution. Differences in composition, structure, and morphology of the nanocrystals, arising from traditional and microwave methods, were studied by several techniques (TEM, Fourier transform infrared spectroscopy (FTIR)-attenuated total reflectance (ATR), dynamic light scattering (DLS), electrophoretic light scattering (ELS), thermogravimetric analysis (TGA), X-ray diffraction (XRD)), and the extraction yields were calculated. Fine tuning the microwave treatment variables, it was possible to realize a simple, cost-effective way for faster materials’ preparation, which allowed achieving high-quality CNCs, with a defined hydrodynamic diameter (150 nm) and zeta potential (−0.040 V), comparable to those obtained using conventional heating, in only 90 min instead of 16 h.

Processes ◽  
2020 ◽  
Vol 8 (9) ◽  
pp. 1190 ◽  
Author(s):  
Saleem Ethaib ◽  
Rozita Omar ◽  
Siti Mazlina Mustapa Kamal ◽  
Dayang Radiah Awang Biak ◽  
Salah L. Zubaidi

The utilization of biomass waste as a raw material for renewable energy is a global concern. Pyrolysis is one of the thermal treatments for biomass wastes that results in the production of liquid, solid and gaseous products. Unfortunately, the complex structure of the biomass materials matrix needs elevated heating to convert these materials into useful products. Microwave heating is a promising alternative to conventional heating approaches. Recently, it has been widely used in pyrolysis due to easy operation and its high heating rate. This review tries to identify the microwave-assisted pyrolysis treatment process fundamentals and discusses various key operating parameters which have an effect on product yield. It was found that several operating parameters govern this process such as microwave power and the degree of temperature, microwave absorber addition and its concentration, initial moisture content, initial sweep gas flow rate/residence time. Moreover, this study highlighted the most attractive products of the microwave pyrolysis process. These products include synthesis gas, bio-char, and bio-oil. The benefits and challenges of microwave heating are discussed.


Author(s):  
Veeresh Nayak C ◽  
Ramesh MR ◽  
Vijay Desai ◽  
Sudip Kumar Samanta

In recent years, the near net shape metal injection molding process combines desirable features of plastic injection molding and powder metallurgy processes to gain high strength-to-weight ratio for manufacturing complex-shaped parts. The metal injection molding process consists of mixing, molding, debinding, and sintering. Microwave processing has attracted much attention in global research because of its unique features such as its ability to heat and sinter a wide variety of metals and its significant advantages in energy efficiency, processing speed, and compatibility. Also, it presents few environmental risks and can produce refined microstructures. The injected samples to be sintered are composed of fine tool steel metal powder and binders, stearic acid, paraffin wax, low-density polyethylene, and polyethylene glycol (600). In recent years, microwave-assisted post-treatment is considered a novel method for processing green parts. In this work, the green parts are subjected to high-intensity microwave fields which operate at a frequency of 2.45 GHz. Metal injection molding compacts were sintered using multi-mode microwave radiation. The sintering of a metal injection molding compact by microwaves has hardly been reported. The metal injection molding compact showed better results than those produced by sintering with conventional heating. This study evaluates the effect of conventional sintering and microwave sintering on mechanical properties. By optimizing the sintering process, increased sintered hardness, a more homogeneous microstructure, and greater shrinkage were obtained using microwave-assisted sintering.


2020 ◽  
Vol 10 (1) ◽  
Author(s):  
Nur Atiqah Mohamad Aziz ◽  
Robiah Yunus ◽  
Hamidah Abd Hamid ◽  
Alsultan Abdul Kareem Ghassan ◽  
Rozita Omar ◽  
...  

AbstractMicrowave-assisted synthesis is known to accelerate the transesterification process and address the issues associated with the conventional thermal process, such as the processing time and the energy input requirement. Herein, the effect of microwave irradiation on the transesterification of palm oil methyl ester (PME) with trimethylolpropane (TMP) was evaluated. The reaction system was investigated through five process parameters, which were reaction temperature, catalyst, time, molar ratio of TMP to PME and vacuum pressure. The yield of TMP triester at 66.9 wt.% and undesirable fatty soap at 17.4% were obtained at 130 °C, 10 mbar, sodium methoxide solution at 0.6 wt.%, 10 min reaction time and molar ratio of TMP to PME at 1:4. The transesterification of palm oil-based methyl ester to trimethylolpropane ester was 3.1 folds faster in the presence of microwave irradiation. The total energy requirement was markedly reduced as compared to the conventional heating method. The findings indicate that microwave-assisted transesterification could probably be an answer to the quest for a cheaper biodegradable biolubricant.


2019 ◽  
Vol 16 (3) ◽  
pp. 194-201 ◽  
Author(s):  
Renu Bala ◽  
Vandana Devi ◽  
Pratibha Singh ◽  
Navjot Kaur ◽  
Pawandeep Kaur ◽  
...  

Background: Tetrahydroindazole, a member of the fused-pyrazole system, is a least studied class of heterocyclic compounds owing to its scarcity in nature. However, a large number of synthetically prepared tetrahydroindazoles are known to show a variety of biological activities such as interleukin- 2 inducible T-Cell kinase inhibitors, AMPA receptor positive allosteric modulators, antitumor, antituberculosis, anti-inflammatory and antimicrobial activities. Vilsmeier-Haack reaction is one of the most important chemical reactions used for formylation of electron rich arenes. Even though Vilsmeier- Haack reaction was studied on a wide variety of hydrazones derived from active methylene compounds, literature lacks the examples of the use of 4-substituted cyclohexanones as a substrate for the synthesis of 4,5,6,7-tetrahydroindazoles. The study of the reaction of Vilsmeier-Haack reagent with hydrazones derived from cyclic keto compounds having active methylene has been considered the interested topic of investigation. In the present study, ethyl cyclohexanone-4-carboxylate was treated with one equivalent of various hydrazines for two hours and the resulted hydrazones were further treated with an OPC-VH reagent (Vilsmeier-Haack reagent isolated from phthaloyl dichloride and N,Ndimethylformamide) afforded 4,5,6,7-tetrahydroindazoles in excellent yields. The synthesized compounds 4a-f and 5a-f were screened for their antioxidant activities using the DPPH radical scavenging assay. The target compounds were synthesized regioselectively using 4+1 approach in excellent yields. A number of experiments using both conventional heating as well as microwave irradiation methods were tried and on comparison, microwave irradiation method was found excellent in terms of easy work up, high chemical yields, shortened reaction times, clean and, no by-products formation. Some of the synthesized compounds showed significant antioxidant activity. The microwave assisted synthesis of 4,5,6,7-tetrahydroindazoles from ethyl cyclohexanone-4-carboxylate has been reported under mild conditions in excellent yield. Easy work up, high chemical yield, shortened reaction times, clean and no by-products formation are the major advantages of this protocol. These advantages may make this method useful for chemists who are interested in developing novel 4,5,6,7-tetrahydroindazole based drugs.


2019 ◽  
Vol 16 (2) ◽  
pp. 117-121 ◽  
Author(s):  
Peipei Han ◽  
Wenhua Zhou ◽  
Mingxia Chen ◽  
Qiuan Wang

A series of eight polymethoxychalcone Mannich base derivatives 2a-2h was synthesized via the microwave-assisted Mannich reaction of natural product 2'-hydroxy-3,4,4',5,6'-pentamethoxychalcone (1) with various secondary amines and formaldehyde. Compared to conventional heating method (80°C), the microwave-assisted method (700W, 65°C) is efficient with short reaction time (0.5-1 h) and good yields (74-88%). The antiproliferative activities of eight Mannich base derivatives were evaluated in vitro on a panel of three human cancer cell lines (Hela, HCC1954 and SK-OV-3) by CCK-8 assay. The results showed that all of the Mannich base derivatives exhibited potential antiproliferative activities on tested cancer cell lines with the IC50 values of 9.13-48.51 µM. Some active compounds exhibited more activity as compared to positive control cis-Platin. Among them, compound 2b revealed to have the strongest antiproliferative activity against all the three cancer cell lines with IC50 values ranging from 9.13 to 11.24 µM.


2020 ◽  
Vol 7 (3) ◽  
pp. 183-195
Author(s):  
Musa Özil ◽  
Emre Menteşe

Background: Benzoxazole, containing a 1,3-oxazole system fused with a benzene ring, has a profound effect on medicinal chemistry research owing to its important pharmacological activities. On the other hand, the benzoxazole derivative has exhibited important properties in material science. Especially in recent years, microwave-assisted synthesis is a technique that can be used to increase diversity and quick research in modern chemistry. The utilization of microwave irradiation is beneficial for the synthesis of benzoxazole in recent years. In this focused review, we provide a metaanalysis of studies on benzoxazole in different reaction conditions, catalysts, and starting materials by microwave technique so far, which is different from conventional heating. Methods: Synthesis of different kind of benzoxazole derivatives have been carried out by microwave irradiation. The most used method to obtain benzoxazoles is the condensation of 2-aminophenol or its derivatives with aldehydes, carboxylic acids, nitriles, isocyanates, and aliphatic amines. Results: Benzoxazole system and its derivatives have exhibited a broad range of pharmacological properties. Thus, many scientists have remarked on the importance of the synthesis of different benzoxazole derivatives. Conventional heating is a relatively inefficient and slow method to convey energy in orientation to the reaction medium. However, the microwave-assisted heating technique is a more effective interior heating by straight coupling of microwave energy with the molecules. Conclusion: In this review, different studies were presented on the recent details accessible in the microwave- assisted techniques on the synthesis of the benzoxazole ring. It presents all examples of such compounds that have been reported from 1996 to the present. Benzoxazoles showed an extensive class of chemical substances not only in pharmaceutical chemistry but also in dyestuff, polymer industries, agrochemical, and optical brighteners. Thus the development of fast and efficient achievement of benzoxazoles with a diversity of substituents in high yield is getting more noteworthy. As shown in this review, microwave-assisted synthesis of benzoxazoles is a very effective and useful technique.


2018 ◽  
Vol 27 (4) ◽  
pp. 096369351802700 ◽  
Author(s):  
Mehmet Önal ◽  
Gökdeniz Neşer

Glass reinforced polyester (GRP), as a thermoset polymer composites, dominates boat building industry with its several advantages such as high strength/weight ratio, cohesiveness, good resistance to environment. However, proper recovering and recycling of GRP boats is became a current environmental requirement that should be met by the related industry. In this study, to propose in a cost effective and environmentally friendly way, Life Cycle Assessment (LCA) has been carried out for six scenarios include two moulding methods (namely Hand Lay-up Method, HLM and Vacuum Infusion Method, VIM) and three End-of-Life (EoL) alternatives(namely Extruding, Incineration and Landfill) for a recreational boat's GRP hulls. A case study from raw materials purchasing phase to disposal/recycling stages has been established taking 11 m length GRP boat hull as the functional unit. Analysis show that in the production phase, the impacts are mainly due to the use of energy (electricity), transport and raw material manufacture. Largest differences between the methods considered (HLM and VIM) can be observed in the factors of marine aquatic ecotoxicity and eutrophication while the closest ones are abiotic depletion, ozon layer depletion and photochemical oxidation. The environmental impact of VIM is much higher than HLM due to its higher energy consumption while vacuum infusion method has lower risk than hand lay-up method in terms of occupational health by using less raw material (resin) in a closed mold. In the comparison of the three EoL techniques, the mechanical way of recycling (granule extruding) shows better environmental impacts except terrestrial ecotoxicity, photochemical oxidation and acidification. Among the EoL alternatives, landfill has the highest environmental impacts except ‘global warming potential’ and ‘human toxicity’ which are the highest in extrusion. The main cause of the impacts of landfill is the transportation needs between the EoL boats and the licenced landfill site. Although it has the higher impact on human toxicity, incineration is the second cleaner alternative of EoL techniques considered in this study. In fact that the similar trend has been observed both in production and EoL phases of the boat. It is obvious that using much more renewable energy mix and greener transportation alternative can reduce the overall impact of the all phases considerably.


Molecules ◽  
2021 ◽  
Vol 26 (10) ◽  
pp. 2882
Author(s):  
José Miranda de Carvalho ◽  
Cássio Cardoso Santos Pedroso ◽  
Matheus Salgado de Nichile Saula ◽  
Maria Claudia França Cunha Felinto ◽  
Hermi Felinto de Brito

Luminescent inorganic materials are used in several technological applications such as light-emitting displays, white LEDs for illumination, bioimaging, and photodynamic therapy. Usually, inorganic phosphors (e.g., complex oxides, silicates) need high temperatures and, in some cases, specific atmospheres to be formed or to obtain a homogeneous composition. Low ionic diffusion and high melting points of the precursors lead to long processing times in these solid-state syntheses with a cost in energy consumption when conventional heating methods are applied. Microwave-assisted synthesis relies on selective, volumetric heating attributed to the electromagnetic radiation interaction with the matter. The microwave heating allows for rapid heating rates and small temperature gradients yielding homogeneous, well-formed materials swiftly. Luminescent inorganic materials can benefit significantly from the microwave-assisted synthesis for high homogeneity, diverse morphology, and rapid screening of different compositions. The rapid screening allows for fast material investigation, whereas the benefits of enhanced homogeneity include improvement in the optical properties such as quantum yields and storage capacity.


e-Polymers ◽  
2021 ◽  
Vol 21 (1) ◽  
pp. 200-209
Author(s):  
Caiyun Zhang ◽  
Chunhong Li ◽  
Bolin Ji ◽  
Zhaohui Jiang

Abstract A fast, simple, and energy-saving microwave-assisted approach was successfully developed to prepare carbon microspheres. The carbon microspheres with a uniform particle size and good dispersity were prepared using glucose as the raw material and HCl as the dehydrating agent at low temperature (90°C) in an open system with the assistance of microwave heating. The carbon microspheres were characterized by elemental analysis, XRD, SEM, FTIR, TG, and Raman. The results showed that the carbon microspheres prepared under the condition of 18.5% (v/v) HCl and heating for 30 min by microwave had a narrow size distribution. The core–shell structure of the carbon core and TiO2 shell was prepared with (NH4)2TiF6, H3BO3 using the microwave-assisted method. The hollow TiO2 microspheres with good crystallinity and high photocatalytic properties were successfully prepared by sacrificing the carbon microspheres.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Dawei Zhang ◽  
Lihong Zhang ◽  
Bingzhe Wang ◽  
Guangzhe Piao

Stable lyotropic chiral nematic liquid crystals (N*-LCs) of cellulose nanocrystals (CNs) were prepared via hydrolysis using sulfuric acid. The lyotropic N*-LCs were used as an asymmetric reaction field to synthesize polyaniline (PANI) onto CNs by in situ polymerization. As a primary step, we examined the mesophase transition of the N*-LCs of CNs suspension before and after in situ polymerization of aniline (ANI) by polarizing optical microscopy. The structure of nanocomposites of PANI/CNs was investigated at a microscopic level using Fourier transform infrared spectroscopy and X-ray diffraction. Influence of the CNs-to-ANI ratio on the morphology of the nanocomposites was also investigated at macroscopic level by scanning electron and transmission electron microscopies. It is found that the weight ratio of CNs to aniline in the suspension significantly influenced the size of the PANI particles and interaction between CNs and PANI. Moreover, electrical properties of the obtained PANI/CNs films were studied using standard four-probe technique. It is expected that the lyotropic N*-LCs of CNs might be available for an asymmetric reaction field to produce novel composites of conjugated materials.


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