Progress in the Study of Microwave Pyrolysis Technology and Its Influencing Factors

In recent years, the effective conversion of organic wastes into valuable products has been a focus and difficulty in sustainable energy and environmental management. Organic wastes come from a wide range of sources, and industrial and agricultural sources are the main sources of organic waste in China, which can be controlled by microwave pyrolysis technology. In microwave pyrolysis treatment, catalysts have been the key material, microwave absorber, and catalyst of the research hotspot in recent years. This paper summarises the typical influencing parameters of microwave pyrolysis (including microwave power, pyrolysis temperature and microwave absorber), and also summarises the various catalysts applied in microwave pyrolysis, and looks forward to the potential application prospect of pyrolysis products, and the future development direction.

Mass-Based Environmental Factor and Energy Assessment of Microwave-Assisted Synthesized Transition Metal Nanostructures

This paper describes mass-based energy phase-space projection of microwave-assisted synthesis of transition metals (zinc oxide, palladium, silver, platinum, and gold) nanostructures. The projection uses process energy budget (measured in kJ) on the horizontal axes and process density (measured in kJg−1) on the vertical axes. These two axes allow both mass usage efficiency (Environmental-Factor) and energy efficiency to be evaluated for a range of microwave applicator and metal synthesis. The metrics are allied to the: second, sixth and eleventh principle of the twelve principle of Green Chemistry. This analytical approach to microwave synthesis (widely considered as a useful Green Chemistry energy source) allows a quantified dynamic environmental quotient to be given to renewable plant-based biomass associated with the reduction of the metal precursors. Thus allowing a degree of quantification of claimed “eco-friendly” and “sustainable” synthesis with regard to waste production and energy usage.

Low temperature microwave-assisted vs conventional pyrolysis of various biomass feedstocks

A comparison between conventional pyrolysis and a novel developed low-temperature microwave-assisted pyrolysis methodology has been performed for the valorisation of a range of biomass feedstocks including waste residues. Microwave pyrolysis was found to efficiently deliver comparable evolution of bio-gases in the system as compared with conventional pyrolysis at significantly reduced temperatures （120-180 ℃vs 250-400 ℃）. The gas obtained from microwave-assisted pyrolysis was found to contain CO2, CH4 and CO as major components as well

Preparation of lithium carbonate by microwave assisted pyrolysis

Investigations were conducted to purify crude Li_(2)CO_(3)via direct carbonation with CO_(2)at atmospheric pressure and pyrolysis with both water bath heating method and microwave heating method.The reaction kinetics of LiHCO_(3)pyrolysis was studied and the effect of different operating conditions including initial concentration of LiHCO_(3)solution,pyrolysis temperature and stirring speed on the purity of Li_(2)CO_(3)was investigated to obtain the optimal operating conditions.Results showed that the effect law is similar in the two pyrolysis processes.The purity of the Li_(2)CO_(3)increases firstly and then decreases with the increase of the initial concentration of LiHCO_(3)solution and the stirring speed,while the purity of Li_(2)CO_(3)first decreases and then increases with the increase of pyrolysis temperature.The product yield increases with the increase of initial concentration of LiHCO_(3)solution and pyrolysis temperature and is essentially unaffected by the stirring speed.Under the optimal operating conditions,the purity of Li_(2)CO_(3)can reach up to 99.86%and 99.81%in water bath heating and microwave heating process,respectively.In addition,the pyrolysis rate of microwave assisted pyrolysis is 6 times that of water bath heating process,indicating that the microwave heating technology can significantly improve pyrolysis efficiency and reduce energy consumption.

Conversion of Biomass to Hydrocarbon-rich Bio-oil via Microwave-assisted Catalytic Pyrolysis： A Review

The method for pyrolysis of biomass to manufacture hydrocarbon-rich fuel remains challenging in terms of conversion of multifunctional biomass with high oxygen content and low thermal stability into a high-quality compound, featuring high content of hydrocarbons, low oxygen content, few functional groups, and high thermal stability. This study offers a promising prospect to derive hydrocarbon-rich oil through microwave-assisted fast catalytic pyrolysis by improving the effective hydrogen to carbon ratio(H/Ceff) of the raw materials. The proposed technique can promote the production of high-quality bio-oil through the molecular sieve catalyzed reduction of oxygenated compounds and mutagenic polyaromatic hydrocarbons. This work aims to review and summarize the research progress on microwave copyrolysis and microwave catalytic copyrolysis to demonstrate their benefits on enhancement of bio-oils derived from the biomass. This review focuses on the potential of optimizing the H/Ceff ratio, the microwave absorbent, and the HZSM-5 catalyst during the microwave copyrolysis to produce the valuable liquid fuel. This paper also proposes future directions for the use of this technique to obtain high yields of bio-oils.

Microwave-Assisted Au and Ag Nanoparticle Synthesis: An Energy Phase-Space Projection Analysis

Microwave-assisted synthesis of gold and silver nanoparticles, as a function of Green Chemistry, non Green Chemistry, and four applicator types are reported. The applicator types are Domestic microwave ovens, commercial temperature controlled microwave chemistry ovens (TCMC), digesters, and axial field helical antennae. For each of these microwave applicators the process energy budget where estimated (Watts multiplied by process time = kJ) and energy density (applied energy divided by suspension volume = kJ·ml-1) range between 180 ± 176.8 kJ, and 79.5 ± 79 kJ·ml-1, respectively. The axial field helical field an-tenna applicator is found to be the most energy efficient (0.253 kJ·m-1 per kJ, at 36 W). Followed by microwave ovens (4.47 ± 3.9 kJ·ml-1 per 76.83 ± 39 kJ), and TCMC ovens (2.86 ± 2.3 kJ·m-1 per 343 ± 321.5 kJ). The digester applicators have the least energy efficiency (36.2 ± 50.7 kJ·m-1 per 1010 ± 620 kJ). A comparison with reconstructed ‘non-thermal’ microwave oven inactivation microorganism experiments yields a power-law signature of n = 0.846 (R2 = 0.7923) four orders of magnitude. The paper provides a discussion on the Au and Ag nanoparticle chemistry and bio-chemistry synthesis aspects of the microwave applicator energy datasets and variation within each dataset. The visual and analytical approach within the energy phase-space projection enables a nanoparticle synthesis route to be systematically characterized, and where changes to the synthesis are to be mapped and compared directly with historical datasets. In order to help identify lower cost nanoparticle synthesis, in addition to potentially reduce synthesis energy to routes informed changes to potentially reduce synthesis energy budget, along with nanoparticle morphology and yield.

Green Chemistry Allometry Test of Microwave-Assisted Synthesis of Transition Metal Nanostructures

Microwave irradiation is considered an important approach to Green Chemistry, because of its ability to rapidly increase the internal temperature of polar-organic compounds that lead to synthesis times of minutes rather than hours when compared to conventional thermal heating. This works describes a dual allometry test for the discrimination between the solvents and reagents used in the microwave-assisted synthesis of transition metal (zinc oxide, palladium silver, platinum, and gold) nanostructures. The test is performed in log-log process energy phase-space projection, where the synthesis data (kJ against kJ·mol-1) has a power-law signature. The test is shown to discriminate between recommended Green Chemistry, problematic Green Chemistry, and Green Chemistry hazardous solvents. Typically, recommended Green chemistry exhibits a broad y-axes distribution within an upper exponent = 1 and lower exponent = 0.5. Problematic Green Chemistry exhibits a y-axes narrower distribution with an upper exponent = 0.94 and lower exponent = 0.64. Non-Green Chemistry hazardous data exhibits a further narrowing of the y-axes distribution within upper exponent = 0.87 and lower exponent = 0.66. In all three cases, the y-axes is aligned to original database power-law signature. It is also shown that in the x-axes direction (process energy budget) the grouped order of magnitude decreases from four orders for recommended Green Chemistry solvent and reagent data, through two orders for non-Green Chemistry hazardous material and down to one order for problematic Green Chemistry.

Microwave-Assisted Transition Metal Nanostructure Synthesis: Power-Law Signature Verification

A power-law (y = cxn) signature between process energy budget (kJ) and process energy density (kJ·ml-1) of microwave-assisted synthesis of silver and gold nanostructures has been recently described [Law and Denis. AJAC, 14(4), 149-174, (2023)]. This study explores this relation further for palladium, platinum, and zinc oxide nanostructures. Parametric cluster analysis and statistical analysis is used to test the power-law signature of over four orders of magnitude as a function of six microwave applicator-types metal precursor, non-Green Chemistry synthesis and claimed Green Chemistry. It is found that for the claimed Green Chemistry, process energy budget ranges from 0.291 to 900 kJ, with a residual error ranging between −33 to +25.9 kJ·ml-1. The non-Green Chemistry synthesis has a higher process energy budget range from 3.2 kJ to 3.3 MJ, with a residual error of −33.3 to +245.3 kJ·ml-1. It is also found that the energy profile over time produced by software controlled digestion applicators is poorly reported which leads to residual error problematic outliers that produce possible phase-transition in the power-law signature. The original Au and Ag database and new Pd, Pt and ZnO database (with and without problematic outliers) yield a global microwave-assisted synthesis power-law signature constants of c = 0.7172 ± 0.3214 kJ·ml-1 at x-axes = 0.001 kJ, and the exponent, n = 0.791 ± 0.055. The information in this study is aimed to understand variations in historical microwave-assisted synthesis processes, and develop new scale-out synthesis through process intensification.

Influence of carbon coating prepared by microwave pyrolysis on properties of LiNi_(1/3) Mn_(1/3) Co_(1/3) O_2

A novel synthesis method of carbon-coated LiNil/3Mnl/3COl/302 cathode material for lithium-ion battery was reported. The carbon coating was produced from a precursor, glucose, by microwave-pyrolysis method. The prepared powders were characterized by scanning electron microscopy （SEM）, X-ray diffraction （XRD）, X-ray fluorescence （XRF） and charge/discharge tests. XRD results indicate that the carbon coating does not change the phase structure of LiNil/3Mnl/3C01/302 material. SEM results show that the surface of spherical carbon-coated material becomes rough. Electrochemical performance results show that the carbon coating can improve the cycling performance of LiNii/3Mnl/3C01/302. The specific discharge capacity retention of the carbon-coated LiNi1/3Mnt/3Col/30z reached 85.0%-96.0% at the 50th cycle at 0.2C rate, and the specific discharge capacity retention is improved at a high rate.

Dielectric and physico-chemical behavior of single thermally thick wood blocks under microwave assisted pyrolysis

Pyrolysis of thermally thick beech wood blocks with a size of around 2.5×8×6 cm^(3)(width×length×height)was carried out in a lab scale microwave reactor with a frequency of 2.45 GHz,operated,both,at 300 W and 600 W under inert conditions,using N_(2) at around 400 mbar absolute pressure.The microwave cavity had a size of 20×20×20 cm^(3).The specific energy supply referred to the untreated wood block was 4-8 W/g,with slight variations depending on the initial water content.The mass loss and the reflected microwave power were in-situ monitored during the experiments.The sample surface and chamber temperatures were measured with a pyrometer and a thermocouple,respectively.Physico-chemical and dielectric properties of the produced solids were investigated and compared to those of chars produced under conventional pyrolysis using the same raw materials.It is shown that the complex dielectric permittivity of the solid products changed drastically during the pyrolysis process,with increasing heating properties as the conversion process evolved.This was easily achieved using 60o W without susceptors.However,300 W was not enough to achieve a high conversion degree,independently of the irradiation time.This,together with the physico-chemical analyses of the solids,hinted to the importance of the transport kinetics in thermally thick materials,although further investigationis still required.

Effect of Process Parameters of Microwave Assisted Extraction (MAE) on Polysaccharides Yield from Pumpkin

Process parameters of microwave assisted extraction （MAE） of the polysaccharides from pumpkin viz. extraction temperature, time and liquid-solid ratio were studied by using single factor and response surface methodology method. The results showed that the liquid-solid ratio was the most important factor in polysaccharides yield, followed the extraction temperature was the least important factor. The optimum microwave assisted extraction co by ndi extraction time, and tions for the highest polysaccharides yield from pumpkin （16.76%-4-0.38%） were obtained by using the response surface methodology with extraction time of 29 min, an extraction temperature of 79 ℃ and a liquid-solid ratio of 22 mL·g^-1. Validation experiment result well agreed with predicted value.

Understanding the influence of microwave on the relative volatility used in the pyrolysis of Indonesia oil sands

In this paper, pyrolysis of Indonesian oil sands （lOS） was investigated by two different heating methods to develop a better understanding of the microwave-assisted pyrolysis. Thermogravimetric analysis was conducted to study the thermal decomposition behaviors of lOS, showing that 550 ℃ might be the pyrolysis final temperature. A explanation of the heat-mass transfer process was presented to demonstrate the influence of mi- crowave-assisted pyrolysis on the liquid product distribution. The heat-mass transfer model was also useful to explain the increase of liquid product yield and heavy component content at the same heating rate by two differ- ent heating methods. Experiments were carried out using a fixed bed reactor with and without the microwave irradiation. The results showed that liquid product yield was increased during microwave induced pyrolysis, while the formation of gas and solid residue was reduced in comparison with the conventional pyrolysis. Moreover, the liquid product characterization by elemental analysis and GC-MS indicated the significant effect on the liquid chemical composition by microwave irradiation. High polarity substances （ε 〉 10 at 25 ℃）, such as oxy- organics were increased, while relatively low polarity substances （ε 〈 2 at 25℃）, such as aliphatic hydrocarbons were decreased, suggesting that microwave enhanced the relative volatility of high polarity substances. The yield improvement and compositional variations in the liquid product promoted by the microwave-assisted pyrolysis deserve the further exploitation in the future,

Effect of industrial microwave irradiation on the physicochemical properties and pyrolysis characteristics of lignite

The surface functional groups and pyrolysis characteristics of lignite irradiated by microwave were comparatively studied to evaluate the feasibility of using industrial 915 MHz for lignite drying. The drying kinetics, micro structure, chemical functional groups, re-adsorption properties, and pyrolysis characteristics of the dried coal were respectively analyzed. Results indicated that for typical Chinese lignite studied in this paper, 915 MHz microwave drying was 7.8 times faster than that of the hot air drying. After industrial microwave drying, the sample possessed much higher total specific surface area and specific pore volume than that of air dried sample. The oxygen functional groups and re-adsorption ratio of microwave irradiated coal decreased, showing weakened hydrophilicity. Moreover, during the pyrolysis of the coal dried by hot air and microwave, the yield of tar largely increased from 1.3% to 8.5% and the gas production increased correspondingly. The composition of the tar was also furtherly analyzed, results indicated that Miscellaneous hydrocarbons(HCs) were the main component of the tar, and microwave irradiation can reduce the fraction of polycyclic aromatic hydrocarbons(PAHs) from 26.4% to 22.7%.

The influence of microwave irradiation on rocks for microwaveassisted underground excavation

Demand is growing for explosive-free rock breakage systems for civil and mining engineering, and space industry applications. This paper highlights the work being undertaken in the Geomechanics Laboratory of Mc Gill University to make a real application of microwave-assisted mechanical rock breakage to fullface tunneling machines and drilling. Comprehensive laboratory tests investigated the effect of microwave radiation on temperature profiles and strength reduction in hard rocks(norite, granite, and basalt)for a range of exposure times and microwave power levels. The heating rate on the surface of the rock specimens linearly decreased with distance between the sample and the microwave antenna, regardless of microwave power level and exposure time. Tensile and uniaxial compressive strengths were reduced with increasing exposure time and power level. Scanning electron micrographs(SEMs) highlighted fracture development in treated basalt. It was concluded that the microwave power level has a strong positive influence on the amount of heat damage induced to the rock surface. Numerical simulations of electric field intensity and wave propagation conducted with COMSOL Multiphysics~ software generated temperature profiles that were in close agreement with experimental results.

ITO nano-powders prepared by microwave-assisted co-precipitation in aqueous phase

By using microwave-assisted co-precipitation in aqueous phase, adding surface activation agent PEG-6000 into the mixture of InCl3 solution and SnCl4 solution, and dropping the ammonia solution with the density (volume ratio) of 1-0 to 1-4, ITO precursor was prepared at different reaction system temperatures of 35 ℃-85 ℃, then ITO nano-powder was obtained after it was calcinated at 800 ℃ for 1 h. The morphology of ITO nano-powder was characterized by SEM and its electrical conductivity was determined by conductivity meter. The effects of different temperatures and ammonia concentration in microwave-assisted reaction system on its morphology and electric conductivity were discussed. The experimental results indicate that with the dilution of the ammonia solution or the rise of reacting system temperature, the morphology of ITO particles is transformed from spherical to rod-like one with the decline of its electric conductivity. And the electric conductivity of ITO nano-powders with spherical morphology is higher than that of ITO nano-powders with rod-like morphology.

Efficient recovery of valuable metals from waste printed circuit boards by microwave pyrolysis

The recycling of waste printed circuit board(WPCBs) is of great significance for saving resources and protecting the environment. In this study, the WPCBs were pyrolyzed by microwave and the contained valuable metals Cu, Sn and Pb were recovered from the pyrolyzed WPCBs. The effect of pyrolysis temperature and time on the recovery efficiency of valuable metals was investigated. Additionally, the characterization for morphology and surface elemental distribution of pyrolysis residues was carried out to investigate the pyrolysis mechanism. The plastic fiber boards turned into black carbides, and they can be easily separated from the metals by manual. The results indicate that 91.2%, 96.1% and 94.4% of Cu, Sn and Pb can be recovered after microwave pyrolysis at 700 °C for 60 minutes. After pyrolysis, about 79.8%(mass)solid products, 11.9%(mass) oil and 8.3%(mass) gas were produced. These gas and oil can be used as fuel and raw materials of organic chemicals, respectively. This process provides an efficient and energy-saving technology for recovering valuable metals from WPCBs.

MICROWAVE-ASSISTED EXTRACTION OF GLYCYRRHIZIC ACID FROM LICORICE ROOT-EFFECT OF THE PROPERTY OF SOLUTION ON EXTRACTION OF GA

The property of extraction solution is an important factor influencing the extraction efficiency. In the present work, the effect of the property of solution on extraction of GA was studied, which including the concentration of ethanol, ammonia and cation (M+), pH of extraction solution, different kinds of organic solvent etc. The results show that 50%-60%(v/v) ethanol can reach high percentage extraction of GA. If 1% (v/v) ammonia solution was added into 60%(v/v) ethanol, the percentage extraction can be increased from 2.0% to 2.31%. Without ammonia, 50mmol/L [M+] (M+ = K+, NH4+) was added into 60%(v/v) ethanol, percentage extraction of GA can reach about 2.26%. If pH of solution (60% ethanol) was adjust to pH=4.0, it can reach high percentage extraction. If pH of solution (60% ethanol + 50mmol [M+], pH=6.1) was adjust tO PH=4.0, especially M+ is K+ or NH4+, it can reach almost same extraction efficiency as that of 1% ammonia solution + 60% ethanol, and the operation environment can be greatly improved.

Microwave Assisted Sintering and Photoluminescence Properties of BaaSi6OleNe：Eu^2＋ Green Phosphors

Eu^2＋-doped Ba3Si6012N2 green phosphors were prepared by microwave assisted sintering method at 1275℃ for 4 h, while the counterparts using conventional solid-state reaction method were synthesized at temperature higher than 1300℃ and for to 10 h. Microwave assisted sintering could reduce the activation energy and enhance the diffu- sion rate, thus greatly improved the sintering. Moreover, the influence of Si3N4 content on phase formation, morphol- ogy, absorption, and quantum efficiency, and photoluminescence properties of phosphors were studied. As a result, the Ba3Si6OI2N2：Eu^2＋ samples sintered by microwave assisted sintering method have a higher phase purity and photo- luminescence intensity under ultraviolet excitation as compared with samples sintered in the conventional tube furnace The proposed method is a potential preparation method for the oxynitride phosphors with strong photoluminescence and high phase purity.

Microwave-Assisted Alkaline Pretreatment and Microwave Assisted Enzymatic Saccharification of Oil Palm Empty Fruit Bunch Fiber for Enhanced Fermentable Sugar Yield

Lignocellulosic materials are promising alternative feedstocks for bioethanol production. However, the recalcitrant nature of lignocellulosic biomass necessitates an efficient pretreatment pretreatment step to improve the yield of fermentable sugars and maximizing the enzymatic hydrolysis efficiency. Microwave pretreatment may be a good alternative as it can reduce the pretreatment time and improve the enzymatic activity during hydrolysis. The overall goal of this paper is to expand the current state of knowledge on microwave-based pretreatment of lignocellulosic biomass and microwave assisted enzymatic reaction or Microwave Irradiation-Enzyme Coupling Catalysis (MIECC). In the present study, a comparison of microwave assisted alkali pretreatment was tried using Oil Palm empty fruit bunch. The microwave assisted alkali pretreatment of EFB using NaOH, significantly improved the enzymatic saccharification of EFB by removing more lignin and hemicellulose and increasing its accessibility to hydrolytic enzymes. The results showed that the optimum pretreatment condition was 3% (w/v) NaOH at 180 W for 12 minutes with the optimum component loss of lignin and holocellulose of about 74% and 24.5% respectively. The subsequent enzymatic saccharification of EFB pretreated by microwave assisted NaOH (3% w/v);resulted in 411 mg of reducing sugar per gram EFB at cellulose enzyme dosage of 20 FPU. The overall enhancement by the microwave treatment during the microwave assisted alkali pretreatment and microwave assisted enzymatic hydrolysis was 5.8 fold. The present study has highlighted the importance of well controlled microwave assisted enzymatic reaction to enhance the overall reaction rate of the process.

Microwave-assisted Extraction of Rutin and Quercetin from Flos Sophorae

Three microwave-assisted extraction(MAE) procedures were studied. The first procedure was household microwave oven dynamic extraction(HMODE). The second procedure was special microwave oven bath extraction(SMOBE). The third procedure was microwave resonant cavity dynamic extraction(MRCDE). The results obtained by the three microwave-assisted extraction procedures were compared with those obtained by using traditional Soxhlet extraction. The results indicate that the MAE not only took a shorter time, but also simplified the procedure, and made the extraction a higher yield. At the same time the results obtained by the three MAE procedures were also compared with each other.