Matrix-Material Fabrication Technique and Thermogravimetric Analysis of Banana Fiber Reinforced Polypropylene Composites

From the environmental consideration,it would be very interesting to use natural fibers such as banana,jute or coir as reinforcement materials instead of artificial fibers or any kind of synthetic materials.Natural fibers have many advantages over synthetic ones.Polypropylene banana fiber composites(PPBC)are prepared using untreated and alkali-treated banana fibers at 10-25%by weight of the fiber loading.The thermal properties of polypropylene natural fiber composites are very important for technological uses.Thermogravimetric measurements show that the incorporation of banana fiber into PP enhances the thermal stability of composites containing treated fibers,in comparison with untreated fibers.A composite of biodegradable polypropylene(PP)reinforced with short banana natural fibers was prepared by melt blending followed by a hot press molding system.The thermal properties of matrix materials were studied using thermogravimetric analyzers TGA units.It is observed that the introduction of short banana fibers slightly improved the thermo oxidative stability of PP-banana composites.Physical and chemical changes occurred through dehydration,phase transition,molecular orientation,crystallinity disruption,oxidation and decomposition,and incorporation of several functional groups.Systematic investigations of the thermal behavior of polymers in gas,vacuum or inert atmosphere give the knowledge of how change takes place in polymers.To understand such changes thermogravimetric analysis(TGA)and thermal analysis(TG)were performed.It is observed reinforcement of short banana fiber leads to little improvement in the thermooxidative stability of PPBC.Due to the enhancement of thermo-mechanical properties,such composites may be used as building materials namely roof materials,selling materials and many other engineering applications.

Spontaneous combustion liability between coal seams: A thermogravimetric study

The spontaneous combustion liability of coal can be determined by using different experimental techniques.These techniques are well-known in their application,but no certain test method has become a standard to prove the reliability of all of them.A general characterisation which included proximate and ultimate analyses,petrographic properties and spontaneous combustion tests(thermogravimetric analysis(TGA)and the Wits-Ehac tests)were conducted on fourteen coal and four coal-shale samples.The spontaneous combustion liability of these samples collected between coal seams(above and below)were predicted using the TGA and the Wits-Ehac tests.Six different heating rates(3,6,9,15,20 and 25
C/min)were selected based on the deviation coefficient to obtain different derivative slopes and a liability index termed the TGspc index.This study found that coal and coal-shale undergo spontaneous combustion between coal seams when exposed to oxygen in the air.Their intrinsic properties and proneness towards spontaneous combustion differ considerably from one seam to the other.The Wits-Ehac test results agreed with the TGspc results to a certain extent and revealed the incidents of spontaneous combustion in the coal mines.

Thermogravimetric Analysis of Swine Manure Solids Obtained from Farrowing, and Growing-Finishing Farms

The modern trend of increasing the number of pigs at production sites led to a noticeable surplus of manure. Separation of manure solids provides an avenue of their utility via thermochemical conversion techniques. Therefore, the goal of this paper was to assess the physical and thermal properties of solid separated swine manure obtained from two different farms, i.e., farrowing, and growing-finishing, and to determine their pyrolysis kinetic parameters. Swine manure solids were dried and milled prior to assessing their properties. Differential and integral isoconversional methods (Friedman, and Flynn-Wall-Ozawa) were used to determine the apparent activation energy as a function of the conversion ratio. Significant differences were observed in the proximate, ultimate composition between both manure types. The higher heating value (HHV) for the manure solids from farrowing, and growing-finishing farms reached 16.6 MJ/kg and 19.4 MJ/kg, respectively. The apparent activation energy computed using Friedman and FWO methods increased with the increase in the degree of conversion. Between 10% and 40% degrees of conversion, the average activation energies, using Friedman method, were103 and 116 kJ/mol for the farrowing and growing-finishing manure solids, respectively. On the other hand, the same activation energies, calculated from FWO method, were 98 and 104 kJ/mol, for solid manure obtained from farrowing and growing-finishing farms, respectively. The findings in this study will assist in the effort to optimize thermochemical conversion processes to accommodate swine waste. This could, in turn, minimize swine production impacts on the surrounding ecologies and provide sustainable energy and biochar streams.

Thermogravimetric study of the effect of a PVA oxygen-insulating barrier on the spontaneous combustion of coal

Coal samples in the air for three months were characterized by Thermogravimetric Analysis (TGA). The effect of a PVA oxygen-insulating barrier on the spontaneous combustion of coal was examined. The moisture loss activation energy, oxidation activation energy and combustion activation energy were calculated by an integral method using the Coats-Redfen formula. The results show that the tendency for spontaneous combustion of three coal samples (judged by the activation energy) falls in the order: CYW>YJL>SW. The oxidation activation energy and combustion activation energy of coal protected by the PVA oxygen-insulating barrier increased. A significant increase in the combustion activation energy was noted, especially for the CYW coal where the in-crease was 28.53 kJ/mol. Hence, oxidation of the protected coal samples was more difficult. The PVA oxygen-insulating barrier helps to prevent spontaneous combustion of the coal.

Pyrolysis and combustion kinetics of lycopodium particles in thermogravimetric analysis

Biomass is a kind of renewable energy which is used increasingly in different types of combustion systems or in the production of fuels like bio-oil. Lycopodium is a cellulosic particle, with good combustion properties, of which microscopic images show that these particles have spherical shapes with identical diameters of 31 μm. The measured density of these particles is 1.0779 g/cm2. Lycopodium particles contain 64.06% carbon, 25.56% oxygen, 8.55% hydrogen and 1.83% nitrogen, and no sulfur. Thermogravimetric analysis in the nitrogen environment indicates that the maximum of particle mass reduction occurs in the temperature range of 250-550 ℃ where the maximum mass reduction in the DTG diagrams also occurs in. In the oxygen environment, an additional peak can also be observed in the temperature range of 500-600 ℃, which points to solid phase combustion and ignition temperature of lycopodium particles. The kinetics of reactions is determined by curve fitting and minimization of error.

Evaluation of oxygen uncoupling characteristics of oxygen carrier using micro-fluidized bed thermogravimetric analysis

Oxygen uncoupling characteristics of a natural manganese ore and a perovskitetype oxide CaMn_(0.5)Ti0_(37)5Fe_(0.125)O_(3)were studied by using a microfluidized bed thermogravimetric analysis(MFBTGA)technology which is based on a realtime mass measurement of fluidizing particles inside a bubbling bed reactor.The chemical stability,kinetics of the oxygen release and uptake reactions and fluidization property were investigated and the experimental data measured by MFBTGA were compared with the results in a regular TGA instrument(TGA Q500).The regular TGA Q500 results show the reactivity of both the manganese ore and perovskite oxide are stable for multi cycles,and the oxygen uncoupling capacity of the manganese ore is~1.2%(mass)which is~2 times higher than that of the perovskite oxide.However,the experimental results from the MFBTGA indicated that there is a serious agglomeration for the manganese ore.A very important finding is that the reaction rate of oxygen release and oxygen uptake of the perovskite oxide measured by the MFBTGA are~2 and~4 times faster than that of testedby the TGA Q500.We can conclude that MFBTGA is a very useful tool to measure the reactivity stability and kinetics of oxygen carriers in highthroughput analysis instead of the regular TGA.

Phosphogypsum:Part Ⅰ:Mineralogical,Thermogravimetric,Chemical and Infrared Characterization

Phosphogypsum (PG) derived from the dissolution of phosphate ore in H2SO4 has been characterized by using chemical and thermogravimetric analyses, X-ray difFraction and infrared spectrum to give an idea about the future utifization of this waste material. The PG under the investigation was free from the radioactive elements and Cd and contained about 141 × 10-6 rare earth elements in total, which favours the utilization of this material. PG was formed mainIy of gypsum, little anhydrite and quartz and rare kaolinite. It exhibited two large endothermic peaks corresponding to the dehydration of the sample and a small one which may be attributed to the Iiberation of the residual water that may be found in the soluble anhydrite. Also, an exothermic peak was observed which may be related to the transformation of soluble (γ-anhydrite) to insoluble β-anhydrite. PG exhibited the same absorption bands as that observed for chemical CaSO4.2H2O and natural gypsum samples besides the appearance of a weak band at 840 cm-1 which characterizes the vibration of H2PO4- group

FTIR and Thermogravimetric Analysis of Three Kinds of Nutshells

The main components and pyrolysis characteristics of Camellia oleifera Abel hells, Castanea mollissima Blume shells, and Castanea mollissima Blume shells were analyzed by using FTIR and thermogravimetric methods. The experimental results indicated that the main components of the three kinds of raw materials consisted of cellulose, hemicellulose, and lignin. The highest contents of hemicellulose, cellulose, and lignin were in Camellia oleiferaAbel shells (49.34% ± 0.07%), Castanea mollissima Blume shells (27.34% ± 0.01%), and Carya cathayensis Sarg shells (49.78% ± 0.01%), respectively. The pyrolysis processes of three kinds of shells generally included three stages, namely dehydration, pyrolysis, and carbonization. The peak values and the appearance times of their pyrolysis rates were closely related to their compositions.

Comparative Evaluation of Thermogravimetric and Refractive Index Techniques in Determining Biodiesel Yield

Biodiesel is a clean and renewable resource that consists of mono-alkyl esters of long chain fatty acid, which could be obtained from the transesterification reaction of vegetable oils and animal fats with alcohols and catalysts. Biodiesel yield has typically been determined using expensive and laborious techniques. The attempt of this study was to examine the potential of quantifying the biodiesel conversion in real time using refractive index in transesterification process of canola oil with methanol and KOH. Biodiesel yields at five different mixing intensities and reaction times were measured using a refractometer. The measured results were then compared with analytical data obtained from thermogravimetric analysis (TGA) technique over a temperature range of 25℃ - 600℃. Experimental results indicated that the FAME conversions at different mixing intensity and reaction time measured from refractometer correlated well to the relative weight losses from TGA method with R2 = 0.93 (p ≤ 0.05);however, the refractometer may over-estimate the biodiesel yield when the reaction rate was too low. Overall, the refractometer technique is cheaper and easier to manage and could provide a reliable prediction of biodiesel yield in real time.

Use of Thermogravimetric Analysis for Moisture Determination in Difficult Lyophilized Biological Samples

Residual moisture is a key quality control parameter for lyophilized biologicals, as high moisture can correlate with poor stability. Coulometric Karl Fischer titration is the most widely used technology to determine residual water content;some chemicals are known to cause problems with Karl Fischer titration, but these chemicals do not usually occur in biologics. Three biological samples, of fibrinogen, heparin and Haemophilus influenza b polysaccharide, have caused particular issue in our hands by routine Karl Fischer analysis, illustrating different limitations with this method. The use of thermogravimetric analysis, with evolved gas mass spectrometric monitoring, is described here as a successful alternative for moisture analysis in these materials.

Characterization by Thermogravimetric Analysis of Polymeric Concrete with High Density Polyethylene Mechanically Recycled

This paper presents the results of the characterization by thermogravimetric analysis of a new composite material called polymeric concrete. The polymeric concrete contains micro-particles obtained from High Density Poly-Ethylene (HDPE) mechanically recycled (post-consumer bottles);the official Mexican standard NMX-E-232-SCFI-1999 considers the HDPE as the recyclable plastic material. Thermo-grams based on weight lost were obtained from the raw material (HDPE) and the polymer concrete in order to obtain the glass transition temperature (Tg) and melting temperature (Tf). The analysis conditions were defined from 20°C to 180°C and the heat rate of 1°C/minute. The results show that the glass transition temperature of polymeric concrete is 46°C and the HDPE is 38°C. These results mean that the polymeric concrete is more resistant to decomposition. With respect to the melting temperature, the results show that the 2°C difference between polymeric concrete and HDPE is not significant. The polymeric concrete with HDPE recycled can be considered as composite material thermoplastic. The new material melts when it is heated to 146°C and has the ability to be softened, processed and reprocessed with temperature and pressure changes, which make it possible to obtain molded pieces in the desired shape.

鲍鱼脏器碱提多糖的分离纯化、结构表征及抗氧化活性研究

目的:分离纯化鲍鱼脏器碱提多糖(alkali-extracted abalone vscera polysaccharides,Aavp),并研究其结构和抗氧化活性,以期为鲍鱼脏器碱提多糖的开发及应用提供参考。方法:通过热碱提醇沉获得鲍鱼脏器碱提粗多糖,经DEAE Sepharose Fast Flow和Sephacryl S-400 HR纯化得到高纯度多糖,并利用气相色谱、高效液相色谱、红外光谱和热重分析仪等工具分析其结构及抗氧化活性。结果:粗多糖纯化后得到四个组分,包括Aavp Ia、Aavp Ib、Aavp IIa和Aavp IIb,其中Aavp IIa得率较高,选择其进一步进行结构分析。分析发现,Aavp IIa由木糖和半乳糖组成,分子量为166513 Da;糖苷键构型为α型,组成如下:半乳糖1→4糖苷键摩尔百分比为11.81%,半乳糖1→3糖苷键为34.14%,半乳糖1→2糖苷键为10.14%;木糖1→3糖苷键摩尔百分比为33.85%,1→2和1→4糖苷键共占10.06%。热重分析显示,Aavp IIa在226.4-332.6℃下断裂分解,热失重率为43.65%。抗氧化实验显示Aavp IIa对O2-·的清除率为85.89%,对DPPH·的清除率为62.17%,具有一定的抗氧化活性。结论:提取的鲍鱼脏器碱提多糖是一类杂多糖,并具有一定的抗氧化活性。

热重分析仪样品支架的改进

热重分析仪的样品支架,有可能受到一些特殊样品的分解产物的污染而损坏,为了减少支架污染,扩展仪器的使用范围,增加仪器支架的使用寿命,有必要对热重分析仪的支架进行改进。采用在坩埚底部和样品支架平台之间加铂垫片或氧化铝垫片的方式,对支架进行改进。实验结果表明,添加垫片后对温度的影响可以通过校准进行消除,改进前后一水合草酸钙的测试结果一致。说明仪器支架改进后,仪器的性能没有改变,但是可以有效防止热电偶的损坏或支架与坩埚发生粘连,从而增加仪器的使用寿命和使用范围。

聚苯醚绝缘材料热氧老化动力学参数计算方法

聚苯醚是新能源储能和5G通信等产业领域的重要材料。热重动力学参数计算是快速评定聚苯醚热寿命的关键。但热重分析常选用氮气气氛且升温速率较高,导致老化机理发生改变。为此,该文通过慢速升温和空气气氛下的热重实验模拟聚苯醚的实际老化过程。在多个升温速率对应失效温度区间内拟合温度积分数值解修正Doyle系数,对早期热氧降解阶段进行动力学分析、求取活化能,并推估该阶段反应机理函数以计算指前因子。结果表明,该方法求解活化能的精度较Flynn-Wall-Ozawa法和ASTM E1641-18法更高,且聚苯醚实际热氧老化可等效为遵循类幂律反应机理函数的单一反应,计算得到的指前因子比假定反应机理的标准方法更加可靠。上述工作为聚合物绝缘的热氧老化动力学参数计算提供了有效的技术方法。

孟巴矿高地温环境煤孔隙及氧化动力学特征

为预防高地温煤层开采条件下煤自燃灾害,明确煤的自燃特性,以孟巴矿Ⅵ煤层1306工作面煤样为例,将煤样分别置于40、50、60℃控温炉中恒温处理30天,采用全自动比表面积和孔径分布分析仪测试煤的孔隙结构,利用同步热分析仪测试原煤样和高温预处理煤样的氧化动力学参数。结果表明:孟巴矿煤样经高地温作用后,煤的小孔比例减小,中孔和大孔比例增大,煤样经60℃处理后比表面积由原煤的2.351 m^(2)/g增至3.285 m^(2)/g,总孔容由原煤的0.00788 mL/g增至0.01001 mL/g;与原煤相比,高地温处理后煤样点火温度和燃尽温度显著降低,最大失重量、最大失重速率分别提高6.1%和23.3%;高温处理后煤样的活化能和指前因子均小于原煤,说明高地温环境显著提高孟巴矿煤样的氧化反应活性,增大煤自燃的危险性。

基于热分解的舰用复合材料S2/430LV热工参数

为了研究S2/430LV在热分解前后的热工参数,首先利用热重分析仪对氮气环境中S2/430LV复合材料和430LV树脂进行30~800℃环境下热重试验,分析了两种材料在不同升温速率下热分解响应特征;然后,基于阿伦尼乌斯方程,采用微分法与积分法相结合的方法,确定了S2/430LV热分解动力学参数。研究结果表明:430LV树脂和S2/430LV复合材料在氮气环境中均呈现单一热分解过程,纤维织物会促进430LV树脂基体热分解反应;采用Kissinger方程和Flynm-Wall-Ozawa方程确定S2/430LV活化能取值范围;利用Coats-Redfern方程确定S2/430LV最优热分解机理函数和指前因子,从而建立分解率和温度的函数关系式;采用混合定律,建立了考虑材料分解的热工参数模型。研究结果可为舰艇复合材料结构耐火传热性能研究提供有效数据支撑。

硼砂煅制工艺优化及质量评价

目的 优化硼砂煅制工艺,并对其进行质量评价。方法 以铺设厚度、煅制温度、煅制时间为影响因素,失水率、蓬松度、粉碎率、四硼酸钠含量为评价指标,星点设计-效应面法优化硼砂煅制工艺。采用扫描电镜(SEM)、热重分析(TG)、拉曼光谱、X射线衍射(XRD),比较硼砂煅制前后质量差异。结果 最佳条件为铺设厚度2 cm,煅制温度365℃,煅制时间100 min。煅制后,硼砂微观形态、成分组成、晶型结构发生变化,失去全部结晶水而转变为非晶体状态。结论 该方法稳定可行,可用于工业大批量生产煅硼砂。

发泡聚苯乙烯颗粒流化热解特性的实验研究

基于不同加热速率下的热重测试,计算发泡聚苯乙烯颗粒的热裂解动力学参数,自建可视化流化热解炉研究流化床热解过程,并对产物进行分析。热重实验数据根据阿伦尼乌斯方程用KAS,OFW,CR方法计算活化能和指前因子等热解动力学参数。通过可视化实验观察分析不同温度下发泡聚苯乙烯颗粒热解过程的形态变化,并分析固、液、气三相产物的主要成分。KAS和OFW方法计算的活化能分别为143.55 kJ/mol和147.21 kJ/mol。CR方法计算指前因子为6.79×10^(5)~4.40×10^(8)min^(-1)。发泡聚苯乙烯热解过程中吉布斯自由能为219.30 kJ/mol,反应焓变为137.94 kJ/mol,熵变为-0.12 kJ/K。流化裂解产物主要是苯乙烯、1,3,5-三苯基环己烷、9,9-二甲基萘为主的裂解油、碳黑及甲苯和苯乙烯为主的裂解气。

桂林“鸡血玉”(石英质玉)的稳定性:基于热重分析及红外光谱的探索

中国享有“玉石之国”的赞誉,是世界上最早用玉的国家。角闪石、蛇纹石、绿松石和石英是中国古玉的四种主要材料,50万年前周口店北京人文化遗址中就发现有用玉髓制作的器物[1-2]。桂林“鸡血玉”是中国近20年来开发和应用的一类石英质玉石新品种[3-6],因其独特的红色(又称“黑底红”或“乾坤料”)在外观上可与中国传统珍贵印章石品种之一——鸡血石相媲美,故而得名,但二者在矿物组成、宝石学特征、呈色原理等方面完全不同[4-8]。本研究使用红外光谱仪对采自广西壮族自治区桂林市龙胜县上朗矿区的19块桂林“鸡血玉”(石英质玉)(以下简称“鸡血玉”)样品进行了测试,并选择了7块样品破碎、研磨至200目粉末对其进行热重分析测试(样品基本宝石学特征见表1)。结果显示:(1)“鸡血玉”的主要矿物组成为α-石英。红外光谱中1220~1070 cm^(-1)范围为最强吸收区且有明显分裂峰,由Si-O-Si和Si-O-(Al)非对称伸缩振动产生,特征峰有1218、1176、1170、1076、1072 cm^(-1)。470 cm^(-1)和541 cm^(-1)附近为次强吸收峰区,由O-Si-O弯曲振动所致,470 cm^(-1)处的吸收更强,特征峰有541、540、493、487、470 cm^(-1)。800 cm^(-1)和781 cm^(-1)附近出现肩峰,为Si-O键对称伸缩振动引起,781 cm^(-1)谱峰强度均高于800 cm^(-1),此处的肩峰弱分裂指示“鸡血玉”中SiO 2的晶体粒径较小,属于隐晶质集合体;(2)部分“鸡血玉”样品的红外光谱在1554 cm^(-1)附近出现吸收峰,为水的弯曲振动频率范围,是由水中O的变形振动引起,说明“鸡血玉”样品中含有少量的吸附水;(3)黑地红颜色特征的“鸡血玉”具有不同的热重曲线变化,表明每个样品所含水量与水的分布不尽相同;(4)根据测试样品的TG曲线显示(图1),“鸡血玉”的失重温度范围在200~800℃,主要可分为三个阶段:0~200℃时由于吸附水的流失致使鸡血玉样品最初质量减少;当温度升高至580℃左右,样品的质量变得平稳;在580~800℃范围内“鸡血玉”样品失重较快,温度升至750℃时开始了第二阶段的失重。此阶段由于高温,“鸡血玉”的结构已受到破坏。测试样品失重量范围区间为0.34%~9.69%。上述研究显示,“鸡血玉”的矿物组成主要为α-石英,玉质较为细腻,具有一定量的吸附水,部分“鸡血玉”饰品在日常佩戴和保存过程中,随着时间的增长会出现“起棉”、颜色变浅、透明度降低等现象,很可能与桂林鸡血玉中含吸附水的矿物失水导致结构变疏松有关,但这一现象可逆。

咖啡渣和去油咖啡渣热解特性的试验研究

【目的】研究咖啡渣(spent coffee grounds,SCG)和去油咖啡渣(defatted coffee grounds,DCG)的热解特性并计算其热解动力学参数,分析两者在不同温度下热解三相产物的变化规律,实现废弃咖啡渣的二次利用。【方法】采用管式炉、热重(thermogravimetry,TG)试验和热裂解-气相色谱-质谱联用仪(pyrolysis-gas chromatography mass spectrometer,Py-GC-MS)开展了热解产物分布和热解特性的研究,采用Flynn-WallOzawa(FWO)法计算了热解动力学参数。【结果】热重分析结果表明,SCG和DCG热解可分为4个阶段,主要热解温度范围为200~400℃,并且在300℃左右时失重率最大,升温速率可促进热解反应的进行。动力学计算结果表明,当转化率由0.1提高至0.7时,SCG和DCG的活化能均随之不断升高,转化率由0.7提高至0.9时,两者活化能均随之有所下降;SCG和DCG的平均活化能分别为293.58和307.86 kJ/mol。Py-GC-MS分析表明,SCG主要热解产物包括芳香族、酚类、醛类等化合物,DCG主要热解产物包括醛类、酚类、杂环类、酯类等化合物,在热解阶段,随着热解温度的升高,芳香族、酚类、杂环类化合物相对含量减少,醛类化合物相对含量先增加后减少。管式炉热解试验结果表明,SCG的热解产物中生物油产率较高,DCG的热解产物中焦炭产率较高。【结论】SCG和DCG在合适的温度下进行热解,有利于酚类、芳香族化合物等重要工业原料的回收,实现其高值化利用。