Investigation of microwave energy to cure carbon fiber reinforced phenylethynyl-terminated polyimide composites,PETI-5/IM7

The application of microwave energy to the processing of carbon fiber reinforced phenylethynyl-terminated polyimide composites (PETI-5/IM7) was investigated and evaluated with a variable-frequency microwave furnace. The thermal and physical properties of the composites were measured by dynamic mechanical thermal analysis, thermogravimetric analysis, thermomechanical analysis, and density and composition tests. The mechanical properties were determined by 3-point-bending and short-beam-shear tests at both room temperature and 177 °C. The shear failure surfaces of both microwave- and thermally cured composites were detected with environmental scanning electron microscopy. A comparison of the thermal and microwave processes was conducted to evaluate the advantage of the microwave process. Microwave-cured composites, fabricated under various pressures at the fixed process temperatures, also were investigated. From these studies, it was concluded that microwave energy successfully was used to fabricate PETI-5/IM7 composites with higher glass-transition temperatures (by 11–16 °C) and higher retention in flexural strength, flexural modulus, and shear strength at 177 °C than those fabricated by the thermal process. Furthermore, the microwave processes required only half the time used for the standard thermal process. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 4616–4628, 1999     

Dehydration of sodium carbonate monohydrate with indirect microwave heating

In this study, dehydration of sodium carbonate monohydrate (Na₂CO₃·H₂O) (SCM) in microwave (MW) field with silicon carbide (SiC) as an indirect heating medium was investigated. SCM samples containing up to 3% free moisture were placed in the microwave oven. The heating experiments showed that SCM is a poor microwave energy absorber for up to 6 min of irradiation at an 800 W of microwave power. The heat for SCM calcination is provided by SiC which absorbs microwave. The monohydrate is then converted to anhydrous sodium carbonate on the SiC plate by calcining, i.e. by removing the crystal water through heating of the monohydrate temperatures of over 120 °C. The calcination results in a solid phase recrystallization of the monohydrate into anhydrate. In the microwave irradiation process, dehydration of SCM in terms of indirect heating can be accelerated by increasing the microwave field power.     

Fast Microwave‐Mediated Bulk Polycondensation of d,l‐Lactic Acid

The polycondensation of D ,L ‐lactic acid upon microwave irradiation was studied. The results of polycondensation by means of microwave were compared to those obtained from conventional heating of lactic acid at 100°C, and it was found that the reaction proceeds with much higher rate upon microwave irradiation. The oligomer mixtures formed were investigated by means of matrix‐assisted laser desorption/ionization mass spectrometry (MALDI MS). The molecular mass of the poly(lactic acid) formed under microwave irradiation was found to increase with irradiation time, and the formation of cyclic oligomers after 20 min of reaction time was also revealed.     

Polymerizations of epoxides with microwave energy

The polymerization of the bisaliphatic epoxy resin, 3,4‐epoxycyclohexylmethyl, 3,4‐epoxycyclohexylcarboxylate initiated by diaryliodonium or triarylsulfonium salts under both microwave energy and conventional thermal heating, was investigated. DSC and FTIR methods to determine the extent of polymerization were established. Some polymerization phenomena such as polymerization selectivity, polymerization temperature shift, and polymerization temperature shift by microwave power setting in microwave fields compared to thermal fields were investigated. To explain the phenomena, a theory that a new partition function existed in microwave fields was proposed with statistical thermodynamics. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 4230–4246, 2004     

A study of the effect of the synthesis conditions of titanium dioxide on its morphology and cell toxicity properties

In this study, titanium dioxide nanoparticles (NPs) were synthesized using the home microwave method, and the effect of the microwave irradiation time on the structure of NPs was investigated. In addition, the morphological effect of these NPs on the toxicity of HDMSCs cells was investigated. The crystalline structure and morphology of the NPs were analyzed using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and field emission scanning electron microscopy (FE-SEM); the cytotoxicity was determined by the methyl thiazolyl tetrazolium (MTT) assay. X-ray diffraction analysis revealed that all thin films had a polycrystalline nature with an anatase phase of TiO₂. It was also found that the crystallite size increased with increasing microwave radiation time. The FTIR spectrum showed Ti-O-Ti properties by the peak in the range between 527 and 580 cm^?1. Further, the FE-SEM images showed that the grain size increased with increasing irradiation time. The MTT assay results showed that the accumulation of NPs leads to toxicity.     

微波辐射分散聚合制备单分散聚苯乙烯-g-聚氧乙烯微球

传统乳液聚合、悬浮聚合、分散聚合等方法可制备高分子微球,但微球表面吸附的表面活性剂或稳定剂,以及表面缺少功能性基团等原因,导致微球应用受到限制.大分子单体技术在制备单分散功能性高分子微球方面具有许多优势,以致近年来备受国内外学者关注[1].聚氧乙烯PEO大分子单体参与St的分散聚合中,PEO大分子单体可与St形成PSt-g-PEO两亲接技共聚物,制得的PSt-g-PEO两亲共聚物既是产物也是稳定剂.聚合过程中PEO起着稳定分散作用,解决了传统聚合反应中需要添加稳定剂,以及反应完成后脱除稳定剂的麻烦[2,3].通过含功能基团的大分子单体,…     

微波协同阳离子交换树脂催化合成阿魏酸乙酯

以732型强酸性阳离子交换树脂为催化剂,在微波辐射下用阿魏酸与乙醇酯化合成了阿魏酸乙酯.通过单因素实验,考察了催化剂活化方法对催化剂活性的影响,结果表明,微波法活化阳离子交换树脂的催化性能好.通过单因素实验和正交实验,考察了催化剂用量、醇酸摩尔比、微波辐射时间、微波辐射功率等因素对反应的影响.确定了最佳反应工艺条件:阿魏酸0.1mol,酸醇摩尔比5:1,催化剂用量为反应物质量的35%,微波功率300w,反应时间30min,产率达84.2%.732型树脂催化剂可再生循环使用,重复使用4次,产率不低于80%.     

Chemical Recycling and Liquefaction of Rigid Polyurethane Foam Wastes through Microwave Assisted Glycolysis Process

Glycolysis of polyurethane rigid foams (PUFs) was performed utilizing microwave irradiation at atmospheric pressure. The effects of various metal hydroxide and acetate catalysts as well as different microwave powers were investigated. All reactions were monitored by FTIR spectroscopy. The recovered liquid product containing OH functional groups was applied as a portion of the polyol in formulation of a new polyurethane rigid foam product. The reactivity factors and densities were compared with the foam produced from totally virgin polyol.     

微波辐射下L-氨基酸的快速消旋方法

微波辐射作用下的L-氨基酸消旋反应是一种新的氨基酸消旋方法，具有对环境友好的优点。本文报道了在微波辐射下，以1．Omol／L氢氧化钠水溶液替代有机酸作为反应溶剂，水杨醛为催化剂，水杨醛与L-氨基酸的摩尔比为0．1，L-氨基酸可以快速消旋；消旋反应随微波辐射功率的提高而加快，在600W时已接近最大反应速率。同时也讨论了微波作用下L-氨基酸的消旋反应机理。     

An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides

A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60 °C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC–MS without any clean-up process. The recoveries were in the range of 93.5–104.6%, and the relative standard deviations were lower than 8.7%.     

Microwave mediated hydrogen deuterium exchange: a rapid synthesis of H-substituted benzimidazole

Deuterium aromatic substituted compounds were prepared by microwave irradiation of the parent unlabeled compounds in the presence of deuterium oxide and deuterium chloride. The percentage of deuterium incorporation was investigated under various reaction conditions. A rapid synthesis of ²H-substituted benzimidazole under microwave irradiation is described.     

Hydrolysis of chitosan under microwave irradiation in ionic liquids promoted by sulfonic acid-functionalized ionic liquids

Hydrolysis of chitosan in ionic liquids was carried out under microwave irradiation (MW) using sulfonic acid-functionalized ionic liquids (SFILs) as catalysts. The effect of microwave power, irradiation time, dosage of SFILs and DMSO was investigated by orthogonal tests. Under the optimal reaction conditions, the yield of total reducing sugars (TRS) reached over 90% within 2 min. The viscosity-average molecular weight of degraded chitosan was determined by viscosity method. The structures of the original and degraded chitosan were characterized by Fourier-transform infrared (FTIR) spectra, X-ray powder diffraction (XRD) analysis and carbon-13 nuclear magnetic resonance spectroscopy (¹³C NMR). The influence of microwave power and irradiation time on the TRS and M_v was further studied. This method can dramatically reduce reaction time.     

Microwave processing of TiO2 blocking layers for dye-sensitized solar cells

The microwave heat treatment of blocking layers for dye-sensitized solar cells has been investigated. It has been found that the solar cell efficiencies achieved with microwave heating were considerably higher than those achieved with conventional heating at low temperatures (100°C). This was attributed to microwave heating providing better sintering of the blocking layer and better interfacial contact between the substrate and the TiO₂ layers. These results are promising with regard to the application of microwave heating to the production of dye-sensitized solar cells on flexible polymer substrates.     

Alcoholysis of Poly(l-lactic acid) under microwave irradiation

Chemical recycling of poly(l-lactic acid) (PLLA) by alcoholysis under microwave irradiation was investigated. Reaction rates in ethanol (140-180 °C) and butanol (130-210 °C) were greater under microwave irradiation than under conventional heating. However, because activation energies were almost the same under both conditions, the reaction mechanisms would be the same, but the reaction rates differed due to the reaction frequency factor.     

微波对烯丙基芳醚的Claisen重排反应影响研究

5种烯丙基芳醚衍生物在无溶剂、无催化剂的条件下进行Claisen重排反应,采用了微波加热和常规加热方式,比较了同等温度下微波加热和常规加热反应速率的差异.结果表明微波加热可以显著提高烯丙基苯醚Claisen重排反应的速率.反应温度为190℃时,微波加热下反应速率可提高5～10倍.微波加热是一种无催化剂、高产率的Claisen重排反应的方法.     

柳树河油页岩微波干燥及其对热解特性的影响

在对家用微波炉改造基础上搭建了微波干燥实验台,研究了柳树河油页岩微波干燥特性及对热解特性的影响。结果表明,微波干燥所需的时间为传统干燥所需时间的20%;微波干燥速率要明显大于传统干燥速率;Page模型适用于描写柳树河油页岩微波干燥过程。微波干燥的油页岩同热风干燥后及原样油页岩的热解活化能随转化率的变化曲线基本一致,整体呈先上升后下降的趋势,在转化率为0.7时达到最大值;热解活化能在80~200 kJ/mol变动;微波干燥油页岩热解反应有机质分解段的活化能增加。     

Production of reducing sugar from corn stover by dilute acid hydrolysis co-catalyzed with metal salts under microwave radiation

Acid hydrolysis of corn stover under microwave radiation by adding four metal salt co-catalysts (ferrous sulfate, copper sulfate, zinc sulfate, and manganese sulfate) to produce reducing sugar was investigated. The influences of microwave power, reaction time, sulfuric acid concentration, and co-catalyst concentration on the yield of reducing sugar were studied. The results show that the catalytic effects of ferrous sulfite and copper sulfate are more obvious for the yield of reducing sugar compared with only dilute acid hydrolysis with microwave radiation. Long-time microwave irradiation resulted in secondary hydrolysis, generating small-molecule compounds and decreasing the yield of reducing sugar. The reducing sugar yield was increased by decreasing the hydrolysis reaction time and microwave radiation power. In terms of reducing sugar yield, the four kinds of metal salt co-catalyst act in the order: ferrous sulfate > copper sulfate > sulfuric acid zinc sulfate > manganese sulfate. At concentration of 3.0 %, the best was ferrous sulfate, producing yield of 35.10 %.     

Synthesis of alkyl α‐aminomethyl‐phenylphosphinates and N,N‐bis(alkoxyphenylphosphinylmethyl)amines by the microwave‐assisted Kabachnik–Fields reaction

As a novel extension, the Kabachnik–Fields reaction was applied to the synthesis of alkyl α‐aminomethyl‐phenylphosphinates, and the double phospha‐Mannich reaction was utilized in the preparation of bis(alkoxyphenylphosphinylmethyl)amines. A total of 27 new aminophosphinate derivatives were synthesized by the microwave‐assisted solvent‐free condensation of alkyl phenyl‐H‐phosphinates, paraformaldehyde, and primary or secondary amines. The starting P‐species were also prepared under microwave conditions. The formation of the N‐methylated aminomethyl‐phenylphosphinate by‐products was also investigated.     

Use of ionic liquid and microwave irradiation as a convenient, rapid and eco-friendly method for synthesis of novel optically active and thermally stable aromatic polyamides containing N-phthaloyl-l-alanine pendent group

An efficient, fast and easy method for synthesis of new optically active and thermally stable aromatic polyamides (PAs) containing pendent phthalimide group and l-alanine flexible side spacer using room temperature ionic liquid (RTIL) by microwave irradiation has been investigated. The results found that RTIL efficiently absorb microwave energy, thus leading to a very high heating rate. All the PAs showed excellent solubility and readily dissolved in various organic solvents. Thermogravimetric analysis (TGA) exhibited that polymers were stable, with 10% weight loss recorded above 373 and 418 °C in the nitrogen atmosphere. In order to see the efficiency of microwave irradiation, this method was compared with polycondensation of the same monomers in RTILs using conventional heating.     

Investigation of the species-specific degradation behaviour of methylmercury and ethylmercury under microwave irradiation

The degradation behaviour of methylmercury (MeHg) under microwave irradiation is investigated, as is the (different) degradation behaviour of ethylmercury (EtHg) under similar irradiation. A simple and highly sensitive SPME-GC-pyrolysis-AFS system was used to analyse the aqueous MeHg and EtHg standard solutions after derivatization with sodium tetraphenylborate (NaBPh₄). Samples were irradiated in a microwave digester at microwave powers ranging from 20 to 160 W for durations of 2 to 10 min. The different tolerances towards microwave treatment of the two organomercury species were evident. Practically no degradation was experienced for MeHg for up to 8 minutes of irradiation at 120 W or for up to 4 minutes at 160 W. Significant analyte loss was observed for EtHg after 2 minutes at 40 W of microwave power. Awarded a Poster Prize on the occasion of the European Winter Conference on Plasma Spectrochemistry, February 2005, Budapest, Hungary