预氧化聚碳硅烷纤维的恒温烧结

本文主要针对预氧化聚碳硅烷纤维的恒温烧结过程进行了基础方面的研究。采用XPS、TG -DTG -DTA、IR对预氧化聚碳硅烷原纤维进行标定 ;采用日本精密天平连续跟踪纤维质量变化情况 ,探讨了烧结过程中温度对纤维失重及收缩的影响 ;采用IR、SEM和数码相机分析了纤维恒温烧结过程中微观结构和宏观形貌的变化情况 ,并对预烧结纤维进行了二次烧结     

预氧化聚碳硅烷纤维的恒温烧结

本文主要针对预氧化聚碳硅烷纤维的恒温烧结过程进行了基础方面的研究。采用XPS、TG-DTG-DTA、IR对预氧化聚碳硅烷原纤维进行标定；采用日本精密天平连续跟踪纤维质量变化情况，探讨了烧结过程中温度对纤维失重及收缩的影响；采用IR、SEM和数码相机分析了纤维恒温烧结过程中微观结构和宏观形貌的变化情况，并对预烧结纤维进行了二次烧结。     

聚碳硅烷纤维氧化交联机理的研究

对聚碳硅烷(PCS)原丝在不同氧化交联温度区间生成的逸出产物进行红外、核磁和GC-MAS分析,并结合交联丝的红外分析,推测氧化交联的机理。结果表明,PCS的氧化交联主要是其Si—H氧化生成Si—OH,后者进而彼此缩合生成Si—O—Si交联结构;氧化交联温度高于150℃时,其部分Si—CH3也开始氧化生成Si—OH并进而交联;同时,在氧化交联过程还发生PCS侧链的热裂解,所形成小分子也通过Si—OH彼此结合,形成较大分子,且其分子量随交联温度的提高而提高。因此,要及时排除氧化交联过程废气,以免逸出产物黏附在纤维表面而导致粘结。     

聚碳硅烷树脂性能及应用研究

合成了聚碳硅烷树脂,以该树脂为原料制备了SiC纤维。用电镜、红外光谱、X射线衍射、差热分析、热失重等方法对SiC纤维进行了研究,并对以聚碳硅烷树脂作为浸渍物质涂覆石墨进行了初步研究。     

固/液态聚碳硅烷共混制备碳化硅纤维的研究

以超支化液态聚碳硅烷(LPCS)与固态聚碳硅烷(纯PCS)的共混物作先驱体,熔融纺丝;所得原丝再在热空气气氛中氧化交联,在高温氮气气氛中热裂解,得到碳化硅纤维。研究表明,15%(质量分数)LPCS的加入,可使纯PCS先驱体的纺丝温度,从285℃降低到225℃;纺丝性能和纤维表面质量明显提高;还可以提高氧化交联的效率,降低交联温度,从而减少纤维部分融并、粘结的弊端;虽然纤维的室温力学强度有所降低,但抗氧化性能提高,1400℃氧化交联后,力学性能几乎不变;而纯PCS的力学性能却降为原来的50%。     

含乙烯基的聚碳硅烷的合成

利用聚碳硅烷与甲基乙烯基硅氮烷共混热聚反应 ,制得了含乙烯基的聚碳硅烷。分析了甲基乙烯基硅氮烷的结构 ,讨论了两者共热聚的反应过程 ,研究了制备条件对产物性能的影响。通过熔融纺丝制得了含不同乙烯基的适于电子束辐照的聚碳硅烷纤维。     

异型截面聚碳硅烷纤维的制备

以聚碳桂烷为原料,运用三叶型纺丝组件,通过熔融纺丝,制备出了异型截面聚碳硅烷纤维。研究了纺丝温度、压力、牵伸速度对纤维异形度和当量直径的影响,确立了异型截面聚碳硅烷纤维的溶融纺丝工艺。     

连续聚碳硅烷纤维断裂机理与可纺性研究

分析PCS纤维的特点以后 ,讨论PCS熔融纺丝时的纤维断裂机理以及PCS的可纺性影响因素。研究表明 :强度低且非常脆 ,是聚碳硅烷纤维最显著的特点 ;PCS纤维成形时一般不会发生毛细波断裂 ,但极易出现脆性断裂 ;PCS熔体结构粘度指数Δη <0 .2～0 .3时 ,其可纺性较好     

聚碳硅烷制备连续SiC纤维的不熔化处理工艺研究进展

综述了先驱体转化法制备SiC纤维过程中聚碳硅烷(PCS)的各种不熔化处理方式及其发展状况.通过不熔化方式对终烧产物SiC纤维性能的比较,讨论了各种不熔化方式的优缺点及其对SiC纤维中氧含量的影响,并指出了制备高性能SiC纤维不熔化技术研究的国内外差距及发展趋势.     

聚碳硅烷纤维的辐照氧化联合热处理研究

空气气氛下采用γ射线辐照处理聚碳硅烷(Polycarbosilane,PCS)纤维,再于N2气氛下进行热处理.研究了辐照氧化及热处理过程中PCS纤维的质量、化学结构、凝胶含量的变化及热分解特性,分析了热处理对纤维不熔化的影响.研究表明:有氧辐照过程中,PCS纤维增重明显,到1.0 MGy时增重可达16.6％.经热处理后...     

插层化合物在膨化过程中的热分解动力学

采用红外傅立叶变换光谱仪与热重分析仪联动装置在线检测HNO3-CH3COOH—GIC、H2SO4-GIC及H2SO4-CH3COOH—GIC等插层石墨的相变及热分解过程，同时通过快速扫描得到相应时间段内分解产物的红外光谱，并运用Kissinger—Ozawa原理计算了几种典型膨化反应的动力学参数。研究结果揭示了膨化过程的热分解机理，当升温速率在20℃／min～80℃／min范围时，由实验数据计算出膨化反应表观活化能不大于120kJ／mol。     

凝胶前驱体纤维热分解还原制备铁纤维

以柠檬酸铁为原料,通过水溶液中的聚合反应合成了具有良好可纺性的前驱体溶胶,经过干法纺丝、凝胶化和高温热分解还原,制得了直径约为10~15μm的金属铁纤维.本文研究了不同原料、配比、pH值对溶胶前驱体可纺性的影响,应用傅里叶红外光谱(FTIR)、X射线衍射(XRD)和扫描电镜(SEM)对溶胶前驱体的形成、热分解转化过程及产物的物相组成进行了研究.     

聚碳硅烷的挤出胀大与Y型SiC纤维的异形度

研究了聚碳硅烷(PCS)熔体在Y型喷丝孔中的挤出胀大机理、膨胀模型以及膨胀比对Y型碳化硅纤维异形度的影响.结果表明:采用圆形喷丝孔时PCS的膨胀比为1.02～1.15,Y型喷丝孔时膨胀比为1.02～1.43,在与圆形喷丝孔成形条件相当的情况下,Y型喷丝孔的膨胀比比圆形孔的高出约15%,Y型口模周边的剪切应力分布不均、剪切应力内外差异和区域差异是造成其膨胀比增大的根本原因.PCS熔体温度降低或软化点提高,其出口挤出胀大效应增大.由于模口膨胀的影响,Y型PCS纤维的异形度比喷丝孔异形度下降10%～20%.     

柠檬酸镍制备金属镍纤维热分解过程研究

以柠檬酸和碱式碳酸镍为原料,采用溶胶-凝胶法制备柠檬酸镍前驱体纤维,在Ar气气氛下热分解得到金属镍纤维。通过FE-SEM/EDS、DSC-TG、XRD、FT-IR和XPS对金属镍纤维的形貌、前驱体的热分解过程及纤维的物相组成进行表征。结果表明柠檬酸镍前驱体纤维在300℃热处理时出现金属Ni,且热分解过程中没有氧化镍出现。故金属镍纤维是由前驱体直接热分解形成,不经过氧化镍热还原过程。     

Research on the thermal decomposition and kinetics of byproducts from MgO wet flue gas desulfurization

This paper was aimed at the thermal decomposition and kinetics of the byproducts from MgO flue gas desulfurization. The effects of particle size and charcoal on thermal decomposition of the byproducts were investigated by the thermogravimetric analysis method, and the non-isothermal kinetic parameters of the byproducts were evaluated with the Coats–Redfern method. The results showed that the mass loss increased with the decrement of the particle size. However, the effect of the particle size on the mass loss of each thermal decomposition stage was different. Increasing the amount of charcoal powder in the byproducts had an obvious effect on the temperature characteristics of the thermal decomposition of magnesium sulfate, resulting in a reduced thermal decomposition temperature which could facilitate the thermal decomposition process. The equations G(α) = 1−(1−α)^1/2, G(α) = [−ln(1−α)]², and G(α) = 1−(1−α)^1/3 were the quite appropriate kinetic mechanisms describing the thermal decomposition process of MgCO₃, MgSO₃, and MgSO₄, respectively.     

快速烧结法制备连续碳化硅纤维

通过熔融纺丝，不熔化处理制得连续聚碳硅烷（ＰＣＳ）不熔化纤维，采用快速烧结方法制备出性能较好的连续ＳｉＣ纤维。探讨了气封条件的选择，以及烧结速度对ＳｉＣ纤维的组成，结构及性能的影响。结果表明，快速烧结条件下，可以实现向纤维上施加张力以及纤维的无机化转变，烧结速度加快会降低纤维的Ｃ／Ｓｉ（原子比），同时有利于提高纤维的抗拉强度和热稳定性。     

Structure-solubility relationship and thermal decomposition of furosemide

Furosemide, a high ceiling diuretic, decomposes on heating and is very sparingly soluble in water. The aim of this study was to identify the thermal decomposition product(s) of furosemide and to calculate the activation energy needed for this reaction. This was done to gain a better understanding of the unusually low water solubility of this drug. The main thermal decomposition product was identified by nuclear magnetic resonance (NMR), mass spectrometry (MS), and infrared (IR) analysis as 4-chloro-5-sulfamoylanthranilic acid (saluamine), and the activation energy, calculated from thermogravimetric analysis (TGA) measurements, for this reaction was 47.7 (±1.93) kcal/mol. The experimentally measured activation energy was well below the normal 59 ± 4 kcal/mol needed for the cleavage of the C-N bond to form saluamine. This could possibly be explained by the weakening of the C-N bond through the I-effect of the furane ring and the delocalization of the electrons of the aniline nitrogen in the chlorosulfamoyl benzoic acid entity of furosemide. This decomposition of furosemide indicates the breaking of intramolecular bonds before those of intermolecular bonds (separation of individual furosemide molecules). Strong inter- and intramolecular bonds are a probable cause for the poor water solubility of furosemide because, when some of the inter- and intramolecular bonds that form part of the hydrogen bond network disappeared, as in the structurally related decomposition product saluamine, the aqueous solubility increased.     

Study on thermal decomposition characteristics of AIBN

It is found that the results such as observed in the differential scanning calorimeter (DSC), which show the major thermal decomposition (TD) of a self-reactive material, lack the detail to reveal what happens at the initial stage of a reaction. The reaction at this stage is corresponding to the handling condition of storage or transportation, often possibly having the potential to be developed to a runaway reaction. This paper examined and compared the thermal behaviors of AIBN at various working conditions in calorimeters and Dewar vessels. The mechanism that affects the initial reaction and self-heating behavior of the given material was clarified. Near its onset decomposition temperature, physical processes, such as sublimation or melting interfered the initial reaction of AIBN. The mutuality of the physical effect and the chemical reaction made AIBN behave differently under different measuring conditions, and as the result, quasi-autocatalysis or TD possibly occurs in the same sample at the handling temperature range. The heat accumulation storage tests in two Dewar vessels presented completely different self-heating behaviors due to this mechanism and heat transfer capability of the vessels.     

Kinetics of thermal decomposition of organic binders in molds

A set of experiments on determination of the parameters of the gas release from a mold have been performed. The thickness of the casting, the thickness of the mold wall, the process time, and the temperature of the charged metal (liquid gray cast iron) were varied. The investigated molding sands were prepared from quartz sand and organic binders: M19-62 (urea resin), FF-1S (furanic resin), and PK-104 (phenolic resin). On the basis of the experimental data obtained the kinetic parameters of the thermal decomposition of the considered resins have been determined. Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 82, No. 1, pp. 92–97, January–February, 2009.