Vilsmeier-Haack Reagent： Synthesis of 2-Chloro-3-Formyl-1,8-Naphthyridine and Transformation into Different Functionalities

A simple and regioselective synthesis of 2-chloro-3-formyl-l,8-naphthyridine （1） through V ilsmeier-Haack cyclization of N-（pyridine-2-yl） acetamide has been reported. The reaction of compound （1） with sodium sulphide gives thione （2） and the reaction of compound （1） with Na2S/DMF followed by reaction with alkyl halide in one pot afforded thioether （3 and 4）. New naphthyridone （5） was synthesized from the action of acetic acid and POCI3 in compound （1）. The condensation of compounds （1 and 8） with hydroxylamine and aniline leads to the formation of compounds （6, 7 and 9）. The 2-chloro-3-formyl-l,8-naphthyridine was treated with sodium azide underwent cyclization to afford tetrazolo （l,5-a） （l,8-naphthyridine-4-carbaldehyde （8）. The azitidinone （10 and 12） and thioazolidinone （11 and 13） were synthesized from shift base intermediates by using chloroacetyl chloride and thioglycolic acid. The formyl group in compound （1） is subjected to cyano （14） and 3-alkoxycarbonyl （15）, respectively. The ester （15） was treated with hydrazine hydrate in ethanol to give acid hydrazide （16） then converted to thio semicarbazide （17） by their reaction with ammonium thiocyanate. New thiadiazolo （18）, triazolo （19） and oxadiazolo （20） have been prepared. The structures of synthesized compounds have been confirmed by suitable spectroscopic techniques such as IR （infrared spectrometry） and ^1H NMR （proton nuclear magnetic resonance）.     

《江汉石油科技》1998年通讯员名单

韩瑞民（物探处） 彭国斌（物探处） 李海金（采研院） 罗永宽（采油厂） 吴国民（井下作业处） 刘春华（盐化厂） 韦林波（测井处） 赵全福（设计院） 胡江华（钻井处） 胡敏（石化厂） 江子明（四机厂） 李尧初（仪表厂）     

Novel Thermally-Accessible Structural Changes of Chiral and Some Related Cu（ll） Complexes

A mononuclear chiral copper（ll） complex, [Cu（RRchxn）2（C（CN）3）2]＇H20 （RRchxn = （1R, 2R）-diaminocyclohexane） （RRchxnH）, and its deuterated compound, [Cu（RRchxn）2（C（CN）3）z].D20 （RRchxnD）, and their isomers, [Cu（trchxn）2（C（CN）3）2]＇H20 （trchxn = trans-l,2-diaminocyclohexane） （trchxnH） and [Cu（trchxn）2（C（CN）3）2]＇D20 （trchxnD） have been prepared and characterized by means of 1R （infrared）, electronic, and CD （circular dichroism） spectra, magnetic susceptibility, and variable-temperature X-ray crystallography as single crystals or powder. Interestingly, depending on grain size of samples, RRchxnH exhibits the monoclinic form and the orthorhombic form, which are distinguished by systematic absence and powder XRD （X-ray diffraction） patterns clearly. Although single crystals did not exhibit phase transition, powder XRD patterns of RRchxnH and weakly hydrogen bonded RRchxnD emerged low-temperature phase of monoclinic in the orthorhombic patterns only around 200-220 K. However, as a control, powder XRD patterns of both trchxnH and trchxnD did not exhibit such phase transition clearly.     

Synthesis of N-Substituted （Z）-3-（ （2-Benzyl）-4-Ox opent-2-yl） Pyrrole-2,5-Diones （Maleimides）

A series of N-substituted （Z）-3-（（2-benzyl）-4-oxopent-2-yl）pyrrole-2,5-diones were synthesized and characterized. The compounds were synthesized from dimethyl-2-（（Z）-2-（benzylamino）-4-oxopent-2-en-3-yl） fumarate （9） and dimethyl acetylenedi-carboxylate followed by reaction with some amines in refluxing ethanol. The identification of the compounds were based on spectroscopic analysis such as 1R （infrared）, UV （ultraviolet）, ^1H-NMR （nuclear magnetic resonance） and the microanalysis of the elements （CHN （microanalysis）） data.     

Synthesis and properties of soluble poly（aryl ether sulfone ether ketone）s copolymers containing pendant methyl groups

A series of Poly（arly ether sulfone ether ketone）s containing pendant methyl groups were synthesized by the reaction of 4,4＇-[sulfonylbis （1,4-phenylene）dioxy] dibenzoyl chloride （SODBC） with 4,4＇- diphenoxy diphenylsulfone （DPODPS）, 4,4＇- di（2-methylphenoxy） diphenylsulfone （o-Me-DPODPS）, 4,4＇- di（3-methylphenoxy） diphenylsulfone （m-Me-DPODPS）, 4,4＇- di （2,6-bimethylphenoxy） biphenylsulfone（o-Me2-DPODPS） respectively, in a mixture of 1,2-dichloroethane （DCE） and N-methylpyrrolidone （NMP）. These reactions were catalyzed by anhydrous aluminum chloride （AlCl）. The characteristic of copolymers were studied by means of advanced analytical techniques such as FT-IR,1H-NMR, DSC, TGA and WAXD. The results show glass transition temperature （Tg） in the range of 193-206℃, thermally stable in excess of 434℃ and excellent solubility in polar solvents. Methyl-substituted Poly（aryl ether sulfone ketone）s had higher glass transition temperatures, lower initial decomposition temperatures than the unsubstituted ones.     

《江汉石油科技》1997年度优秀通讯员名单

谢维肖（测井所） 陈红桥（物探处） 韩瑞民（物探处） 赵全福（设计院） 赵东昌（钢管厂） 李海金（采研院） 李名泉（钻井处） 吴江（钻头厂） 江子明（四机厂） 马道秀（机械所） 臧波（环保农林处） 罗永宽（采油厂）     

多种Rh配合物在1-辛烯中活化的原位红外研究

应 用 原 位 红 外 光 谱 技 术, 研 究 了 Ｒｈ （ ａｃａｃ） （ Ｃ Ｏ） （ Ｐ Ｐｈ３） 、 Ｈ Ｒｈ （ Ｃ Ｏ） （ Ｐ Ｐｈ３） ３ 、 Ｒｈ ６ （ Ｃ Ｏ） １６ 和（ Ｒｈ（ Ｃ Ｈ３ Ｃ Ｏ Ｏ） ２）２４ 种催化剂,在 Ｃ Ｏ／ Ｈ２ 气氛中催化１ 辛烯氢甲酰化 反应时 Ｒｈ 催化剂的活 化过程。结果表明,在以 Ｏ Ｐ Ｐｈ３ 为配体的情况下,催化剂的中间体均为 Ｗｉｌｋｉｎｓｏｎ 型配合物 Ｈ Ｒｈ（ Ｃ Ｏ）ｘ（ Ｏ Ｐ Ｐｈ３） ｙ（ ｘ ＋ ｙ ＝ ３ 或４） ,此外,同时还存在有二聚体、多羰基铑配合物等。当４ 种催化剂在无配体的情况下,醛化反应的活性仍然较高,此时观察到在使用（ Ｒｈ（ Ｃ Ｈ３ Ｃ Ｏ Ｏ） ２） ２ 及 Ｒｈ ６（ Ｃ Ｏ）１６ 时, 最终生 成 Ｈ Ｒｈ（ Ｃ Ｏ）４ 的活性中 间体。当使 用 Ｒ Ｈ（ａｃａｃ） （ Ｃ Ｏ） （ Ｐ Ｐｈ３） 及 Ｈ Ｒｈ（ Ｃ Ｏ）（ Ｐ Ｐｈ３） ３ 时,活性中间体仍然以 Ｈ Ｒｈ（ Ｃ Ｏ）ｘ（ Ｐ Ｐｈ３） ｙ 型配合物为主,同时可能存在少量的 Ｈ Ｒｈ（ Ｃ Ｏ） ４ 中间物。     

Preparation of High Molecular Weight Poly（L-lactide-co-caprolactone）（75/25）

P（LLA-CL）（75/25） （poly（L-lactide-co-caprolactone）（75/25）） was synthesized from high purity L-lactide and e-caprolactone using tin octoate as initiator by ring-opening polymerization, and characterized by infrared spectrum and ^1-NMR （^1H proton spectrum of nuclear magnetic resonance） spectrum. The synthesized P（LLA-CL）（75/25） is a random copolymer. The influences of polymerization temperature, polymerization time and dosage of initiator on the weight average molecular weight and the polydispersity index of P（LLA-CL）（75/25） were investigated. The optimum preparation condition of P（LLA-CL）（75/25） was： the polymerization pressure is less than 0.5 Pa, the polymerization temperature is 125℃, the n（M）/n（I） ratio is 8,000/1, the polymerization time is 36 h. Under the condition, the weight-average molecular weight of prepared P（LLA-CL）（75/25） is 45.3×10^4, and molecular weight distribution coefficient is 1.24.     

《江汉石油科技》1996年度通讯员名单

李海金（油田处） 江子明（四机厂） 谢维肖（测井所） 刘春华（盐化厂） 方世良（钻井处） 郭先茂（绿化处） 韦林波（测井处）     

新场地区须二段泥岩稀土元素地球化学特征及意义

为了探讨川西坳陷新场地区须二段的物源、沉积环境及源区构造背景,对研究区泥岩的稀土元素（REE）地球化学特征进行了系统分析,结果表明：研究区样品的稀土元素总量较高;w（∑LREE）／w（∑HREE）,（w（La）／w（Yb））N和（w（Ce）／（w（Yb））N的比值表明轻重稀土分异明显;REE配分模式显示为明显的轻稀土元素（LREE）富集、重稀土元素（HREE）平坦型,Eu为明显的负异常,Ce为正常型。6Ce与占Eu．（w（∑REE）的相关性表明成岩作用对研究区泥岩样品的REE特征有一定的影响：δCe δSCe及（w（La）／w（Ya））。值表明研究区水体相对较浅,沉积速率较慢,属相对低能的弱氧化环境。根据稀土元素组合及其比值特征,认为研究区源岩主要为沉积岩和花岗岩;源区构造背景为活动大陆边缘,     

《石油化工》学术指导委员会

主任委员　　袁晴棠　（工程院院士,中国石油化工集团公司）副主任委员　　毛炳权　（工程院院士,北京化工研究院）委员（以姓氏笔画为序）万惠霖　（科学院院士,厦门大学化学系）闵恩泽　（科学院、工程院院士,石油化工科学研究院）何鸣元　（科学院院士,石油化工科学研究院）林励吾　（科学院院士,中科院大连化学物理研究所）彭少逸　（科学院院士,中科院山西煤炭化学研究所）邓景发　（科学院院士,复旦大学化学系）余国琮　（科学院院士,天津大学化工系）胡永康　（科学院院士,抚顺石油化工研究院）侯虞钧　（科学院院士,浙江…     

Anisotropic Lattice Strain of Composite Materials of LiMnO2 and H/D-Substituted Chiral Cyanide-Bridged Ni（Ⅱ）-Fe（Ⅲ） Coordination Polymers

Composite materials composed of LiMnO2, a typical electrode material for lithium ion battery, and a chiral cyanide-bridged Ni（Ⅱ）-Fe（Ⅲ） coordination polymer [NiL2][Fe（CN）6]·4H2O （Ni-Fe, H-form） （L = （1R,2R）-（-）-1,2-cyclohexane-diamine） or its deuterium isomer, [NiL2][Fe（CN）6]·4D2O （Ni-Fe, D-form） have been prepared by the various ratios （w/w） of Ni-Fe：LiMnO2 = 10：0 （pure Ni-Fe）, 9：1, 8：2, 7：3, 6：4, 5：5, 4：6, 3：7, 2：8, 1：9 and 0：10 （pure LiMnO2）. Gradual shift of IR （infrared） spectra by changing the ratios and losing difference between H-form and D-form of Ni-Fe due to isotope effects revealed adsorption of Ni-Fe onto LiMnO2 to form composite materials. Formation of composite materials of Ni-Fe and LiMnO2 could be also proved losing ferromagnetic behavior of LiMnO2 on increasing of the ratios of Ni-Fe in each composite. In contrast to smoothly positive thermal expansion of pure LiMnO2 along the crystallographic b axis, variable temperature powder XRD （X-ray diffraction） patterns at 100-300 K of the composite materials exhibited thermally-accessible lattice distortion along the b axis with different ratios. It is also proved deviation of ideal linear correlation of an evaluation function, In K = a/T ＋ b （where, K = （d（T） - d（0））/d（T）, d（T） denotes nλ/（sin 2θ） at T （K））.     

Nano Fibrous Cerium（IV） Hydrogen Phosphate Membrane Self Supported Indole Polymerization Agent

Nanosized fibrous cerium（IV） hydrogen phosphate membrane, Ce（HPO4）2·2.9H20 （nCePf）, was prepared and characterized by chemical, XRD （X-ray diffraction）, TGA （thermogravimetric analysis）, SEM （scanning electron microscopy） and TEM （transmission electron microscopy）. Novel supported nanofibrous Ce（IV） phosphate/polyiondole nanocomposite membranes were prepared via in-situ chemical oxidation of the monomer that was promoted by the reduction of Ce（IV） ions present in the inorganic matrix. The presence of Ce（IV） ions allows redox reactions necessary to oxidative polymerization to occur. The resultant material was characterized by TGA, elemental （C, H, N） analysis and FT-IR （Fourier transform spectroscopy）. SEM images of the resulting nanocomposite reveals a uniform distribution of the polymer on the inorganic matrix. Amount of polyindole polymer present in the composite is found to be - 7.0%.     

Effect of sample treatment on determination of arsenic （Ⅲ） and arsenic （Ⅴ） in aqueous and tissue samples by hydride generation atomic absorption spectrometry

The purpose of this procedure was to optimize and improve a method that used for the determination of arsenic （Ⅲ） and arsenic （Ⅴ） in biological and environmental samples. The method is based on hydride generation and atomic absorption spectrometry. For both As （Ⅲ） and As （Ⅴ） the parameters such as NaBH4, HCI concentration, and pH were optimized. Absorption signal of As （Ⅴ） was approximately 17% of As （Ⅲ） signal. Therefore, for estimation of As （Ⅲ） and As （Ⅴ） concentrations in various samples the difference between the absorbance obtained for arsenic, without and with previous treatment of samples with potassium iodide （KI）, can be applied. The calibration graphs were linear （r〉0.99）, and the detection limits of the method based on three times the standard deviation of the blank were 0.14 and 0.64 μL^-1 for As （Ⅲ） and As （Ⅴ）, respectively. The relative standard deviation （R.S.D.） of measurements was less than 10%. As a means of checking performance method, water samples were spiked with known concentrations of both As （Ⅲ） and As （Ⅴ）, and recovery above 94% was obtained. The proposed method was applied successfully to determine inorganic As （Ⅲ） and As （Ⅴ） in various environmental and total As in biological samples.     

焦化柴油催化氧化吸附脱硫工艺条件优化

以磷钼酸季铵盐为催化剂,三氟乙酸为氧化剂,糠醛为萃取剂,采用催化氧化-萃取吸附组合工艺对焦化柴油进行脱硫处理。结果表明,在反应温度为60℃,氧化剂用量（V（氧化剂）/V（焦化柴油））为0.2,催化剂用量（m（催化剂）/V（焦化柴油））为8 g/L,反应时间为60 min,萃取剂用量（V（萃取剂）/V（焦化柴油））为1.0,萃取时间为30 m in的最佳工艺条件下,焦化柴油的硫质量分数可从1.05×10-3下降为42×10-6。     

《江汉石油科技》2006年优秀通讯员

马春莲（江汉采油厂） 彭国斌（物探研究院） 曾梅（地球物理勘探公司） 袁明前（测录井工程公司） 方琴（钻井工程公司） 刘春华（盐化工总厂）     

聚丙烯树脂组合物、树脂成型部件及其生产方法

聚丙烯树脂组合物含有2至15wt％成型性改进剂（A）和85至98wt％聚丙烯树脂（B）。该成型性改进剂（A）由丙烯嵌段共聚物（A-1）和（A-2）形成。丙烯嵌段共聚物（A-1）和（A-2）的每-个具有结晶丙烯聚合物组分（A-11）、（A-21）和丙烯-乙烯无规共聚物组分（A-12）、（A-22）。该丙烯嵌段共聚物（A—1）特征在于结晶丙烯聚合物组分（A-11）的熔体流动速率高，而丙烯嵌段共聚物（A-2）特征在于丙烯-乙烯无规共聚物组分（A-22）的含量比高。该聚丙烯树脂（B）由丙烯-乙烯嵌段共聚物（B—1）、     

航空润滑油高温沉积物抑制剂的应用研究

研究高温沉积物抑制剂是提高航空润滑油的高温使用效率的要求,评价航空润滑油高温沉积性能的模拟实验方法有：斜板沉积实验（IPDT）和差示扫描量热法（DSC）。含硫羧酸（SCCA）、二巯基噻二唑（DMTD））、巯基烷基醇（MAA）和三聚硫氰酸（TTCU）及其衍生物与三嗪化合物（Triazine）配伍加入到酯类油中,可明显提高油品的抗氧化性能和抑制高温沉积物的形成。     

Biosorption of Chromium from Aqueous Solution Using Chitosan

Adsorption experiment from aqueous solutions containing known amount of Cr （chromium） using chitosan was explored to evaluate the efficiency of chitosan as sorbent for Cr. Some variable parameters such as pH, reaction time and chitosan dosage were optimized. Under the optimum experiment condition, the effect of common ions on the adsorption of Cr （i.e., Na^＋, K^＋, Mg^2＋, Ca^2＋ for Cr（Ⅲ）, and Cl^-, NO3^-, SO4^2- for Cr（Ⅵ）） was also investigated. Furthermore, the sorption mechanism of Cr by chitosan was investigated by applying Langmuir and Freundlich isotherm equations to the data obtained. In addition, to confirm the characteristics of the chitosan, the surface morphology of the biomass was determined by SEM （scanning electron microscope） and specific surface area analyzer （N2-BET （Brunaeur, Emmet and Teller））. Consequently, the following matters have been mainly clarified： （1） chitosan can be an efficient sorbent for Cr （both Cr（Ⅲ） and Cr（Ⅵ））; （2） the effect of common ions on the adsorption ofCr （Cr（Ⅲ） and Cr（Ⅵ）） was not significant under this experimental conditions; （3） adsorption isotherms using the chitosan can be generally described by Langmuir isotherm more satisfactorily for Cr. The adsorption may have occurred mainly by monolayer reaction; （4） the rates of adsorption were found to conform to pseudo-second order kinetics.     

突变理论在煤层气储层评价中的应用——以准噶尔盆地砂沟井田为例

煤层气储层评价的方法较多,但将突变理论应用于该类储层的评价则少见。为此,在分析突变理论原理的基础上,综合考虑A（资源特征）、B（开采性能）、C（煤层特征）、D（构造特征）等因素,根据层次分析法原理,建立由目标层、准则层和指标层组成的煤层气储层评价多层次结构,确定了煤层气储层评价突变模型。其中指标层A1（含气量）、A2（资源丰度）、A3（含气饱和度）构成燕尾突变模型;B1（储层渗透率）、B2（储层压力）、B3（顶板孔隙度）、B4（底板孔隙度）构成蝴蝶突变模型;C1（煤层厚度）、C2（煤级）、C3（灰分）构成燕尾突变模型;D1（构造特征）、D2（水文特征）构成尖点突变模型;准则层A、B、C、D构成蝴蝶突变模型。运用突变理论对新疆准噶尔盆地南部煤田砂沟井田煤层气储层进行了评价,得出砂沟井田煤层气储层中下侏罗统八道湾组（J₁b）第5号煤层最有利,然后依次为第6、8、9、19号煤层。突变理论模型与模糊综合评判结果一致,该方法减少了以往评价模型中人为主观因素,评价方法更简单,评价结果更可靠,为煤层气储层评价提供了一条新途径。