木薯淀粉硫酸酯的制备及理化性质

以NaHSO3和NaNO2为酯化剂,采用水相法制备了低取代度的淀粉硫酸酯(SSE),测定了SSE糊的冻融稳定性、凝沉性能、透明度、黏度;利用红外光谱仪分析了产物的化学结构.结果表明,酯化的SSE糊的透光率比淀粉的提高22.4％,透明度稳定性明显增强;SSE糊的黏度冷热差值均比淀粉的低,抗老化性能增强、凝沉性能得以改善,...     

高取代淀粉磷酸单酯合成的研究

本文对木薯淀粉干法酯化中淀粉乳液的浓度、pH值、Na_2HPO_4和NaH_2PO_4的用量对酯化取代度的影响,并对酯化温度,反应时间、催化剂用量与取代度、粘度的关系作了探讨,确定了合成高取代淀粉磷酸单酯的最佳反应条件。     

机械活化木薯淀粉氧化产物的结构表征

采用搅拌球磨机对木薯淀粉进行机械活化,以活化60min的木薯淀粉为原料,CuSO4为催化剂,H2O2为氧化剂干法制备氧化淀粉。利用红外光谱、扫描电子显微镜、X-射线衍射等手段对产物的结构进行表征分析,并与原淀粉的氧化产物进行比较。结果表明,机械活化对木薯淀粉的氧化反应有显著的影响。原木薯淀粉的氧化反应主要发生在淀粉颗粒的表面及无定形区,部分发生在结晶区,产物是无定形及结晶状态的结构;活化淀粉的氧化反应在淀粉团粒表面及内部均匀进行,产物是无定形的聚集状态结构。并就机械活化对淀粉氧化的强化机理进行了探讨。     

药物控释载体醋酸酯淀粉的消化性能研究

采用生物体外(in-vitro)消化模型模拟人体消化道环境，对不同取代度的醋酸酯化木薯淀粉的消化速率进行了研究；用微生物酶对醋酸酯化木薯淀粉进行生物降解并测定各个样品的抗消化淀粉含量。结果表明醋酸酯化会增大淀粉颗粒的消化速率，但随取代度的提高消化速率呈下降趋势。同样随取代度的提高，醋酸酯化也会降低淀粉糊的消化速率。醋酸酯淀粉卡抗消化淀粉含量低于原淀粉，且取代度越高含量越低。醋酸酯化会破坏和抑制淀粉中抗消化淀粉的形成。     

微细化交联木薯淀粉醋酸酯的制备与研究

本文以三偏磷酸钠为交联剂,醋酸酐为酯化剂,采用先交联、后酯化,先酯化、后交联,两种方案对木薯淀粉进行改性,并对木薯淀粉醋酸酯进行微细化处理。利用IR、SEM、XRD和TGA对合成产物进行表征;并对其冷热粘度进行了研究。结果表明,理想合成路线为:先酯化,后交联合成交联木薯淀粉醋酸酯。通过机械球磨,能有效地将木薯淀粉颗粒微细化,并可通过球磨时间控制淀粉颗粒的粒度和形貌。测试表明,微细化交联木薯淀粉醋酸酯的耐热性下降、结晶度下降;冷粘度增高,但热粘度性质有所下降。     

草酸淀粉酯制备及其性能研究

本文以草酸和玉米淀粉为原料,通过改变原料的摩尔比反应制备了不同取代度(0.1到0.9)的草酸淀粉酯,采用滴定法测定产物的取代度,利用红外光谱和核磁共振表征产物(取代度为0.41)的化学结构,产物中含有羰基的结果表明成功制备了草酸淀粉酯.详细考察了草酸淀粉酯的物理化学性质,利用粘度测定、热重分析、广角X衍射(WXRD)以及湿度吸收等研究不同取代度的草酸淀粉酯的分子量、热稳定性,结晶形态以及吸水性能.结果说明,与玉米淀粉相比,草酸淀粉酯的吸水率随着取代度的提高而增加,其分子量、热稳定性以及结晶性能则呈下降趋势.     

气流超微粉碎对蜡质玉米淀粉结构及理化性质的影响

为探究气流超微粉碎对蜡质玉米淀粉结构及性质的影响,采用扫描电镜、激光粒度分析仪、X-射线衍射仪、红外光谱仪、差示扫描量热仪、快速黏度分析仪等分析手段研究经微细化处理后蜡质玉米淀粉颗粒形貌、晶体结构和理化性质。结果表明,淀粉粒径明显变小,微细化蜡质玉米淀粉粒度中位径减小到6.43μm,粉碎后淀粉颗粒仍为A型结构,颗粒结晶结构被破坏,由多晶态向无定形态转变,粉碎过程淀粉无新的基团产生;热焓值、糊化温度均降低,热糊稳定性好;持水能力增加,冻融稳定性好,微细化蜡质玉米淀粉具有较好的热糊稳定性和冷糊力学稳定性。     

马铃薯淀粉磷酸酯的物理化学特性

通过与玉米淀粉和马铃薯淀粉相比较,研究了马铃薯淀粉磷酸酯（PEPS）的理化特性,包括粘度的测定,热糊与冷糊的稳定性,不同pH值及电解质（NaCl)和非电解质（蔗糖）存在下的粘度曲线,凝胶强度及冻融稳定性,结果表明,马铃薯淀粉磷酸酯比玉米淀粉和马铃薯淀粉具有更优良的热糊与冷糊的稳定性,电解质(NaCl）和非电解质（蔗糖）的存在,对其热糊与冷糊的稳定性基本元影响,凝胶强度高,冻融稳定性好,尤其是耐酸性能强。     

气流超微粉碎对马铃薯淀粉颗粒形貌及理化性质的影响

为探讨气流超微粉碎对马铃薯淀粉颗粒形貌及理化性质的影响,以马铃薯淀粉为原料,利用流化床气流粉碎机在不同分级转速条件下制备超微粉,采用扫描电子显微镜、激光粒度分析仪、X射线衍射仪、快速黏度分析仪、差示扫描量热仪等研究气流超微粉碎对马铃薯淀粉颗粒形貌、颗粒大小及分布、晶体结构、糊化特性、热力学特性、溶解度、膨胀度和冻融稳定性等性质的影响。结果表明,马铃薯淀粉经气流超微粉碎后,淀粉颗粒表面粗糙且有棱角和裂纹,颗粒形状变的不规则,粒度减小且尺寸分布不均,在分级转速3000r/min时颗粒平均粒径由39.75μm减小至13.38μm;粉碎后淀粉粉体松装密度和振实密度降低,压缩度增大;粉碎没有改变淀粉的晶体结构,但结晶度降低;粉碎降低了淀粉糊的衰减黏度和回生黏度,淀粉的热糊及冷糊稳定性较好,降低了淀粉糊化温度和热吸收焓,提高了淀粉溶解度和膨胀度,改变了淀粉冻融稳定性。研究结果为淀粉干法物理改性技术研究和马铃薯淀粉深加工与高值化利用提供理论依据及参考。     

微波辅助酶促月桂酸淀粉酯的合成

以天然玉米淀粉和月桂酸为原料,脂肪酶Novozym 435为催化剂,研究了微波辐照下月桂酸淀粉酯的酶促合成。通过对淀粉进行预处理活化来提高淀粉的酯化反应活性,并主要考察了微波功率、月桂酸用量、脂肪酶Novozym 435用量及反应时间等参数对酶促月桂酸淀粉酯合成的影响。采用气相色谱法进行取代度的测定,并以取代度为考察指标,确定了最佳的反应条件。结果表明,淀粉的最佳预处理方法为NaOH/尿素混合溶液法,经该法处理后淀粉的酯化反应活性大大提高;微波辐照技术的应用大大缩短了反应时间,并提高了月桂酸淀粉酯的取代度。适宜的工艺条件为：微波功率为240W,月桂酸用量为30%,酶加入量为7%,反应时间26min。在上述反应条件下可以制得取代度为 0.0311的月桂酸玉米淀粉酯。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

解决能源问题的新途径——光解水制氢的研究

面对日益枯竭的能源危机,氢能是一种洁净、最有前景的替代能源。目前在各种制氢的方法中光催化分解水制氢的研究最多,光解水过程中催化剂最关键,本文对利用太阳能光解水的途径、提高光催化反应效率以及光催化剂的开发研究进行了综述。