Synthesis and Crystal Structure of 4,4'-(4-(1-Naphthyl)-4-phenyl-1,3-butadienylidene)-bis[N,N-diethylbenzenamine]

The title compound （C40H42N2） has been synthesized by the reaction of l-（l- naphthyl）-l-phenyl-3-chloropropylene and bis（4-（diethylamino） phenyl）methanone, and characterized by IR, ^1H NMR, MS and X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 17.047（3）, b = 10.807（2）, c = 18.494（4） A, β = 105.727（4）°, V= 3279.4（11） A^3, Mr = 550.76, Z = 4, Dc = 1.115 g/cm^3,μ（MoKa） = 0.085 mm^-1, F（000） = 1184, the final R = 0.0625 and wR = 0.1384 for 2276 observed reflections （1 〉 2σ（I））. X-ray analysis reveals that the butadiene fragment adopts a planar cisiod conformation and makes a dihedral angel of 69.4（2）° with the naphthalene ring.

Syntheses and Adsorption Property Research of N-Diethyl Imidazole Modified PS Resins for Iodine

A new N-diethyl imidazole modified PS resins was synthesized in this paper. The composition, structure, and properties of the resulting resins were studied by means of Fourier transform infrared (FTIR) and elemental analysis methods. The results showed that the resins hold the adsorption function group of quaternary ammonium structure. Meanwhile, the adsorption properties of the resulting resins for iodine were investigated. The results showed that the uptake of iodine found to be higher at natural water than at acidic medium;the adsorption capacity increased with the increasing of temperature, but when the temperature is higher than 30°C, adsorption capacity didn’t increase;the adsorption kinetics of the resins can be modeled by pseudo first-order rate equation and pseudo second-order rate equation wonderfully;Both Freundlich equations and Langmuir equations could well interpret the adsorption of resins for iodine.

Synthesis of N,N-diethyl dodecyl amine and its flotation properties on bauxite

N,N-diethyl dodecyl amine(DEN12) was synthesized from dodecyl amine,formic acid and acetic aldehyde.The collecting property of DEN12 on diaspore,kaolinite and illite was investigated by flotation test and infrared spectrum.The results show that in the presence of 2.0×10-4 mol/L DEN12,the recoveries of kaolinite and illite are all higher than 78% and the recovery of diaspore is 50% in the pH range of 5.5-6.0.The mass ratio of Al2O3 to SiO2 in concentrate obtained from separation artificial mixture is higher than 10,suggesting that DEN12 can be used as a collector to separate the aluminosilicates from diaspore in bauxite ores at the pulp pH below 8.The measurements of the infrared spectrum approve that the action between aluminosilicates and tertiary amine collector is strong electrostatic adsorption and that of diaspore is weak electrostatic adsorption.

Lewis acid-oxygen vacancy interfacial synergistic catalysis over SO4^2-/Ce0.84Zr0.16O2-WO3-ZrO2 for N,N-diethylation of aniline with ethanol

Herein,a new mechanism involving Lewis acid-oxygen vacancy interfacial synergistic catalysis fo r aniline N,N-diethylation with ethanol was proposed,and the SO4^2-/Ce0.84Zr0.16O2-WO3-ZrO2 catalyst(SCWZ)with both Lewis acid sites and oxygen vacancies was synthesized by the hydrothermal method,which shows better catalytic activity than the reported solid acidic catalysts.Besides,the SO4^2-/ZrO2(SZ)and SO4^2-/WO3-ZrO2(SWZ)catalysts were also prepared and compared with SCWZ to investigate the synergistic effect of each component.The SO4^2-and WO3 mainly generate Lewis acid by bonding with ZrO2,which is beneficial for the fracture of the N-H bond in aniline.The Ce0.84Zr0.16O2 solid solution mainly plays a vital role in generating the oxygen vacancies as the interface active species,which can participate in stripping-OH from ethanol,then the carbocation will also be released,which only needs1.3805 kcal/mol energy,calculated by density functional theory(DFT),to be input.In comparison,the traditional reaction mechanism needs the Br■nsted acidic sites to promote the protonation of ethanol,then dehydration and subsequent formation of carbocation followed,and 108.6846 kcal/mol energy needs to be input,which is far higher than that of the new mechanism.The apparent activation energy(Ea)over SCWZ was measured by experiment to be 34.09 kJ/mol,which is much lower than that of SWZ(47.10 kJ/mol)and SZ(54.37 kJ/mol),illustrating comparatively preferable kinetics for SCWZ than that of SWZ and SZ.Besides,the conversion of aniline and selectivity to N,N-diethylaniline over SCWZ reach almost 100%and 73%,respectively,The SCWZ can be renewed for 4 times without rapid deactivation,and the longevity of SCWZ is longer than that of SWZ and SZ,as the loaded SO4^2-and tetragonal ZrO2 are stabilized by Ce0.84Zr0.16O2 and WO3,respectively.

Lignans with(N,N-diethyl)methyl amino group from Buxus rugulosa

Buxrugulosides A–E,four lignan glycosides(1–4)and a protocatechuate derivative(5)featuring a rare(N,Ndiethyl)methyl amino group at aromatic rings,were obtained from the aerial parts of Buxus rugulosa,which is famous for treating coronary heart disease.Their structures including absolute configurations were elucidated by HRMS,1 D and 2 D NMR,and by comparing their CD data with previous reports.Compound 1 was a rare sesquilignan,and all of these compounds were the first example of lignans with(N,N-diethyl)methyl amino group.

新型硫氮酯捕收剂的合成及选矿性能研究

以乙硫氮、苯甲酰氯原料,通过取代反应合成出了N,N-二乙基二硫代氨基甲酸苯甲酰酯硫氮酯,考察了物料配比、反应温度、反应时间对产物收率的影响,得出的最佳的工艺条件为:n(C_(5)H_(10)NS_(2)Na·3H_(2)O)∶n(C_(7)H_(5)ClO)=1:1.04,温度为35℃左右,时间120 min条件下合成产率为99.24%,回收率为97.22%以上的N,N-二乙基二硫代氨基甲酸苯甲酰酯硫氮酯产品。将其应用于某铜矿作为捕收剂,与现场药剂相比较,铜精矿铜品位提高1.17%,回收率提高2.25%。将其应用于某铅锌矿作为捕收剂,与异丁基黄药、25#黑药、乙硫氮、丁铵黑药、乙基黄药对比,可以明显提升铅的品位和回收率,同时对硫化锌的捕收力极弱。

N-烷基取代丙烯酰胺共聚体系热敏性质研究

Ｎ烷基取代丙烯酰胺共聚体系热敏性质研究祝黔江（贵州农学院基础部贵阳５５００２５）陶朱马培华刘敏（贵州大学化学系应用化学研究所贵阳５５００２５）关键词共聚Ｎ烷基取代聚丙烯酰胺，浊化温度，浓度，共聚比具有透明白浊热可逆性质的高聚物在三十年前就已有...

羟胺衍生物的辐解研究 ⅡN,N-二乙基羟胺辐解产物中气态烃类的定性定量分析

用三氧化二铝毛细柱与氢火焰离子化检测器联用的气相色谱法,定性定量分析了N,N 二乙基羟胺水溶液辐解产生的气态烃类。结果表明:当吸收剂量为10～1000kGy时,N,N 二乙基羟胺水溶液辐解产生的气态烃类主要有甲烷、乙烷、乙烯、丙烷和正丁烷。甲烷、乙烷、丙烷和正丁烷的体积分数都随吸收剂量的增加而增加;而乙烯的体积分数先是随剂量的增加而增加,当剂量大于500kGy时,其体积分数则随剂量的增加而明显减少。

自来水系统中游离氯检测器的评价

本试验采用2种氯测定仪(Cifec和Seres)连续在线检测水中的游离余氯(Cl2+HClO+ClO-)和游离有效余氯(HClO),所有检测数据均与采用DPD法在555 nm得到的不同质量浓度的次氯酸钠标准曲线进行检验.实验结果表明,氯测定仪可以连续便捷测定自来水中的游离余氯量,这对于水厂处理系统实现全自动化运行及其控制氯投加量有着深远的意义.

N,N-二乙基氨荒酸铋化合物(Et_2NCS_2)_2(NO_3)Bi(NO_3)-Bi(S_2CNEt_2)_2(HOCH_3)的合成及晶体结构

利用硝酸铋和N ,N 二乙基氨荒酸盐反应 ,合成了新型铋的N ,N 二乙基氨荒酸衍生物 (Et2 NCS2 ) 2 (NO3 )Bi(NO3 )Bi (S2 CNEt2 ) 2 (HOCH3 ) .通过元素分析和红外光谱对其结构进行了表征 .用X射线单晶衍射测定了该化合物的分子和晶体结构 .结果表明 ,化合物的晶体为三斜晶系空间群P1—,晶胞参数 :a =0 9880 ( 3 )nm ,b =1 2 778( 3 )nm ,c =3 1993 ( 9)nm ,α =89 888( 4 )° ,β =85 72 8( 4 )° ,γ =89 82 4( 4 )° ,Z =4,V =4 0 2 77( 19)nm3 ,Dc=1 92 5g/m3 ,μ =9 183mm-1 ,F( 0 0 0 ) =2 2 48,R1 =0 0 5 2 5 ,wR2 =0 0 5 46.该化合物中存在 2个不同的铋原子 ,它们分别为配位数 7和 8的畸变五角双锥和十二面体构型 .在晶体中 ,通过相邻分子间的S…S弱相互作用和氢键作用 。

羟胺衍生物的辐解研究 Ⅲ .N ,N -二乙基羟胺辐解产生的氢气和一氧化碳的定性定量分析

用5 分子筛填充柱与热导型检测器联用的气相色谱法,定性定量分析了N,N 二乙基羟胺水溶液辐解产生的氢气和一氧化碳。分析氢气时,以氩气为载气,柱温为85℃,检测器温度为110℃;分析一氧化碳时,以氢气为载气,柱温为50℃,检测器温度为80℃。研究结果表明:氢气的体积分数随着吸收剂量的增加而增加,而与N,N 二乙基羟胺浓度的关系不大;一氧化碳只有在很高吸收剂量时才产生,且体积分数很低。

反相流动注射-分光光度法测定水中痕量余氯的研究

研究并建立了测定水中痕量总余氯和游离余氯的Ｎ，Ｎ－二乙基－１，４－苯二胺（ＤＰＤ）反相流动注射分光光度法。将ＤＰＤ 溶液和ＨＰＯ４２－ －Ｈ２ＰＯ４－ 缓冲溶液（ｐＨ ６．７）的混合液注入试样载流中，再与ＫＩ溶液或硫代乙酰胺溶液流混合，在５１０ ｎｍ 处对反应形成的红色半醌式化合物进行分光光度测定。总余Ｃｌ２和游离余Ｃｌ２质量浓度的线性范围均为０．１～３．２ ｍ ｇ／Ｌ，检出限分别为０．０３５ 和０．０３８ ｍ ｇ／Ｌ，测定频率均为６０ 次／ｈ。本法已用于测定自来水中总余氯和游离余氯。

昆虫驱避剂驱蚊肤宁的高效液相色谱分析

目的 :建立紫外 -高效液相色谱法 ,测定驱蚊肤宁中N ,N -二乙基间甲苯甲酰胺(DEET)的含量。方法 :以YWGC18为反相柱 ,甲醇 -水 ( 2 - 1)为流动相 ,紫外检测波长为 2 5 4nm。结果 :驱蚊肤宁中DEET的回收率为 10 0 .10 % ,RSD为 0 .90 % (n =5 )。结论 :该法简便、快速、准确、可靠 ,适合于产品的质量控制。

新型铜硫浮选分离硫氨酯捕收剂的合成及吸附机理

设计合成一种新型铜硫浮选分离捕收剂:O-异丙基-N,N-二乙基硫代氨基甲酸酯(IPDTC)。先利用密度泛函理论计算IPDTC的电子结构。结果表明,IPDTC比O-异丙基-N-乙基硫代氨基甲酸酯(Z-200)具有更高的最高占据分子轨道能量和更低的电负性。根据相互作用能判据预测IPDTC具有较强的捕收能力。浮选试验表明,IPDTC对黄铜矿和黄铁矿的捕收能力强于Z-200。通过表面张力、吸附量、XPS、FTIR和zeta电位等方法研究捕收剂的浮选机理。研究发现,IPDTC可降低溶液表面张力。IPDTC在黄铜矿表面的吸附能力强于黄铁矿,这与浮选试验结果相吻合。FTIR、zeta电位和XPS结果表明,IPDTC通过形成Cu—S—C键在黄铜矿表面发生较强的吸附作用,但在黄铁矿表面的吸附作用较弱。

DPD分光光度法测定循环水中余氯的改进

针对以N,N-二乙基对苯二胺分光光度法测定循环水中余氯时出现的问题进行了实验研究。结果表明,不同的氯标准溶液、显色剂与水样的加入顺序和显色时间对测定的结果均有干扰。建议采用与水中有效氯存在状态接近的氯标准溶液来绘制标准曲线;采用先加入显色剂后再加入水样的方法来避免次氯酸的漂白作用对测定的干扰。

染发剂中4种p-苯二胺N位取代衍生物的高效液相色谱测定法

建立了高效液相色谱(HPLC)同时测定染发剂中N,N-双(2-羟乙基)-p-苯二胺硫酸盐(DHPD)、N,N-二甲基-p-苯二胺硫酸盐(DMPD)、N,N-二乙基-p-苯二胺硫酸盐(DEPD)、N-苯基-p-苯二胺盐酸盐(PPD)4种p-苯二胺N位衍生物的方法。采用Agilent Eclipse XDB-C18柱(150 mm×4.6 mm,5μm)为固定相,25 mmol/L磷酸缓冲液(pH 6.0,含0.1%的辛烷磺酸钠)和乙腈为流动相,梯度洗脱,流速1.0 mL/min,柱温25℃,进样量20μL,检测波长250 nm和280 nm。各组分的线性范围为0.1～400 mg/L,相关系数r为0.999 2～0.999 9,检出限为18～108 mg.kg-1,定量下限为42～320 mg.kg-1,RSD<10%,加标回收率为83%～115%。该方法具有简便、快速、准确等特点,基本满足实际样品的分析要求。

(N,N′—二乙基)偶氮二异丁脒盐酸盐引发下的丙烯酰胺水溶液聚合

本文研究了(N,N′—二乙基)偶氮二异丁脒盐酸盐引发下丙烯酰胺水溶液聚合的反应动力学。得出了聚合速率方程式为RP=KP[EAIBA]05[AM]。测定了聚合表观活化能。并研究了聚合条件对产物分子量及其分布的影响。利用该引发—聚合体系,获得了相对分子量上千万超高分子量聚丙烯酰胺。

增效复方驱避剂的研制

本文报告一种新的复方增效驱避剂——驱蚊露。采取固定剂与成膜剂相结合的方法,驱避效果明显优于国内生产的类似产品。

K_2CO_3/MgO催化合成碳酸乙丙酯

以K_2CO_3/MgO为固体碱催化剂,正丙醇与碳酸二乙酯(DEC)经液相酯交换合成了碳酸乙丙酯(EPC);用X射线衍射和CO_2程序升温脱附的方法对催化剂进行了表征。表征结果显示,随K_2CO_3负载量的增加,MgO载体的特征衍射峰强度减弱,在K_2CO_3负载量较高时有明显的K_2O晶相出现;K_2CO_3/MgO催化剂上的弱碱性位可能是催化该反应的活性中心。同时考察了K_2CO_3负载量、催化剂用量、反应时间和原料配比对酯交换反应的影响。实验结果表明,K_2CO_3负载量为20%(相对于催化剂的质量分数)的K_2CO_3/MgO催化剂对该反应有较好的催化性能;适宜的反应条件为:催化剂用量为反应物质量的1.00%、反应温度403 K、反应时间4 h、n(DEC):n(正丙醇)=1.0:1.5;在此条件下,DEC的转化率为62.32%,EPC的选择性为83.29%,EPC的收率为51.89%。

N,N-二乙基-N’-氟取代苯甲酰基硫脲应用于镍废水处理研究

利用N,N-二乙基-N’-氟取代苯甲酰基硫脲的强配位性研究了其对废水中镍离子的处理作用,并利用火焰原子吸收法对残留镍离子含量进行测定。结果表明,含Ni(II)500 mg/L的模拟废水,在絮凝剂聚合氯化铝与聚丙烯酰胺存在下,酰基硫脲可在pH 7～8范围内将Ni(II)离子沉淀,且残留镍含量远低于国家排放标准。本方法的优点在于:在接近中性的条件下可将镍离子沉淀完全,处理后的废液可不经调节pH直接排放,沉淀下来的酰基硫脲与Ni(II)离子络合物残渣经过酸处理,可重新释放出镍离子和硫脲沉淀,沉淀剂的回收率达72.1%,降低废水处理成本。