高取代度阳离子淀粉的合成及其降滤失性能

高取代度阳离子淀粉的合成及其降滤失性能;环氧丙基三甲基氯化铵;阳离子淀粉;半干法;钻井液;降滤失剂     

新型有机-无机复合型钻井液降滤失剂的制备及性能

以2-丙烯酰胺基-2-甲基丙磺酸、对苯乙烯磺酸钠和丙烯酰胺为共聚单体,氧化石墨烯为无机改性剂,采用水溶液聚合法制备了一种新型的水基钻井液降滤失剂(LC-1),其结构和性能经IR, GC和TG表征。结果表明:LC-1用量为1.6 wt%时,钻井液体系老化前后的滤失量分别为9.2 mL和9.8 mL,动切力为12.5 Pa和10.4 Pa,动塑比为0.30和0.26,钻井液体系的降滤失性、流变性和耐热性较好。页岩滚动回收两次,回收率大于90%。     

微交联聚合物降滤失剂的合成与性能

针对深井、超深井钻井液体系中的降滤失剂受长时间高温、高矿化度作用易降解的问题，以氮丙啶与3-氯丙烯反应制得-N-烯丙基氮丙啶（ALAI）； ALAI与乙二胺反应制得四烯基交联剂单体（EAAD）； EAAD与丙烯酰胺（AM）和2 丙烯酰胺基-2-甲基丙磺酸（AMPS）发生水溶液自由基共聚反应，合成了微交联共聚物降滤失剂(PAAT)，其结构和性能经¹H NMR, IR和TG-DTG表征。结果表明：PAAT可抗220 ℃高温，在高温、高矿化度条件下可维持钻井液的滤失量与流变性能，API滤失量均低于4.0 mL，高温高压滤失量均小于13.0 mL。     

羟甲基化木质素磺酸盐添加剂对钻井液性能的影响

为了进一步优化木质素磺酸盐作为钻井液处理剂的效能,利用其与甲醛的羟甲基化反应制备了羟甲基化木质素磺酸盐;采用红外光谱仪、X射线粉末衍射仪、扫描电镜等分析了其结构;测定了改性前后的木质素磺酸盐对钻井液流变性、降滤失性、黏土水化膨胀抑制性等性能的影响.结果显示,改性后的羟甲基化木质素磺酸盐的整体结构变化不大,但羟基数量增加,与水的相溶性增强.与木质素磺酸盐相比,羟甲基化木质素磺酸盐在室温下对基浆有较强的提黏作用,经180℃高温老化后降黏、降滤失作用有所增强,形成的泥饼厚度降低,对黏土水化膨胀的抑制作用增强.     

X射线荧光光谱法测定黑龙江省有机碳含量较高样品中的硅、铝、铁等元素

通过事先对有机碳含量较高的样品进行高温灼烧,计算其烧失量,再将灼烧后的样品经专用熔剂熔融制样后,经X射线荧光光谱仪测定,能够有效地去除因有机质含量高导致的分析结果的偏差,而且较湿法化学分析节省时间。实验结果表明,该方法的分析结果与湿法化学分析结果偏差很小,准确度较直接压片分析有了大幅提高。     

甲醛-三氯乙酸沉淀-凯氏定氮法测定牛奶中真蛋白质

提出了一种有效去除三聚氰胺等非蛋白氮干扰的凯氏定氮法测定牛奶中真蛋白质的含量的方法。在5mL样品中加入甲醛3 mL,漩涡混匀1 min,于70℃水浴加热10 min后,加入150g·L-1三氯乙酸溶液5mL沉淀蛋白质,抽滤分离后,应用自动凯氏定氮仪测定沉淀中的蛋白质含量。经配对t检验分析,本法与国家标准方法测定牛血清白蛋白标准溶液中蛋白质含量、与考马斯亮蓝G-250法测定牛奶中真蛋白质含量以及干扰试验中各干扰物添加组与对照组中蛋白质含量的测定结果均无显著性差异。被分离的滤液中干扰物的回收率在98.4%~100%之间。     

X射线荧光光谱法测定高含量有机碳样品中的钾、钠、钙、镁、硅、铝、铁、钛、锰、磷

通过事先对有机碳含量较高的样品于1000℃下灼烧2 h,计算其烧失量,再将灼烧后的样品经Li₂B₄O₇(67%)和LiBO₂(33%)的混合熔剂熔融制样后,经X射线荧光光谱仪测定,能够有效地去除因有机质含量高导致的分析结果的偏差,总体的平均相对误差从11.1%减少到了4.5%,而且较湿法化学分析节省时间。分析结果可与湿法化学分析结果相媲美,准确度较直接压片分析方法有了大幅提高。     

自降解屏蔽暂堵剂PAM/PCL的合成及性能研究

针对生物降解塑料聚己内酯（PCL）耐温性能差、高温条件下降解时间快等缺点,本文以丙烯酰胺（AM）和PCL为主要原料,N,N-亚甲基双丙烯酰胺（MBA）为交联剂、过硫酸铵（APS）和亚硫酸氢钠（SHS）为引发剂、失水山梨糖醇脂肪酸酯（Span-80）和乙基纤维素为分散剂,采用反相悬浮聚合法合成了一种自降解暂堵剂,考察了分散剂、搅拌速度、交联剂、油水比和引发剂对暂堵剂降解时间的影响,确定了暂堵剂最佳合成条件：分散剂用量（质量分数,下同）0.4%、搅拌速度400 r·min^-1、油水比（体积比）8:2、交联剂用量0.8%、引发剂用量0.5%。对暂堵剂的性能进行了评价,实验结果表明：暂堵剂具有较好的耐温耐盐性,耐温可达160 ℃,与钻井液配伍性较好,少量暂堵剂就可以有效降低钻井液的滤失量。砂床封堵实验表明：暂堵剂具有较好的封堵性能,暂堵剂用量为0.5%就可使砂床浸入深度减少6.5 cm。     

层层沉积提高井壁稳定性室内研究

以钠蒙脱土分散液作为模拟钻井液,与支化聚乙烯亚胺聚合物溶液交替流过模拟井壁(硅片),模拟生物矿化过程,进行层层沉积模拟实验。通过原子力显微镜、扫描电镜、红外光谱、X射线衍射等手段跟踪钠蒙脱土/聚乙烯亚胺复合膜的成膜过程,并表征复合膜的形貌、微观结构、化学组成及力学性能。结果表明,钠蒙脱土和聚乙烯亚胺可自发在模拟井壁上形成结构致密的有机/无机复合膜,该复合膜具有明显的层状结构,平均每层厚度约为46.18nm。该复合膜力学性能优良,而且杨氏模量并不随沉积层数的增加而变化。通过动态滤失实验表明,层层沉积改善了滤饼质量,降低了滤失速率以及总的动态滤失量,有助于井壁稳定。     

无机盐对流动注射法测定水中阴离子表面活性剂的抑制效应

采用流动注射法测定水中的阴离子表面活性剂的含量。结果表明,实际样品加标回收率偏低,通过样品成分分析测试发现,影响加标回收率的主要干扰为水中的无机盐,表现为抑制效应。本文通过电导率测试对无机盐的抑制机理进行分析,确定首要抑制因子。在样品和标准溶液中加入过量无机盐可以消除抑制干扰,实验结果表明线性、检出限及样品加标回收率均符合方法要求,能够适用于大批量样品分析的实际工作需要。     

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。     

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.     

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.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

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^-。     

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.

     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.