Infrared spectroscopic study on chemical and phase equilibrium in triethylammonium acetate

Protic ionic liquid (PIL) triethylammonium acetate was prepared by mixing equimolar amounts of acetic acid and triethylamine, and then studied using the combination of the Attenuated Total Reflection Fourier Transform Infrared spectroscopy, in-situ infrared spectroscopy, pH, and conductivity titration measurements. It was found that the equimolar synthesized triethylammonium acetate was separated into two layers, which suggesting that there were both chemical and phase equilibrium in this solution. Molecular species could be directly observed in the IR spectra over the range of 1200-1800 cm-1 and also checked by 1H NMR. Based on analysis, the upper layer was rich in amine with little acid and PIL, and the down layer was rich in PIL with residual acetic acid and amine. And single PIL-rich layer could be separated into two layers again when the mole ratio of newly added triethyamine to the theoretical produced triethylammonium acetate reached 0.12.

嘌吟能离子通道型受体7介导的帕金森大鼠认知功能障碍

目的探讨嘌呤能离子通道型受体7(P2X7R)在帕金森(PD)大鼠认知功能障碍中的作用。方法成年大鼠90只实验分为5组,每组6只大鼠,3个重复,运用6-羟基多巴胺(6-OHDA)制备PD大鼠模型。向PD大鼠注射P2X7R激动剂2,3-腺苷5-三磷酸三乙铵盐(BzATP)和拮抗剂考马斯亮蓝G(CBBG)检测大鼠在水迷宫中的学习记忆能力和疼痛反应,Real-time PCR和Western blotting检测海马组织P2X7的表达情况。结果与正常大鼠相比,PD大鼠学习速度缓慢,记忆能力弱,CBBG提高了PD大鼠的学习记忆能力,BzATP使PD大鼠的学习记忆能力减退;海马组织Real-time PCR结果显示,与对照组相比,P2X7R在海马组织中mRNA表达量最高,CBBG组P2X7R表达量下调,BzATP组P2X7R表达量上调;对P2X7R进行Western blotting检测,与PD组相比,BzATP组P2X7蛋白表达量显著升高,CBBG组P2X7蛋白表达量较低。结论PD大鼠存在认知功能障碍,CBBG可改善PD大鼠的学习记忆功能,BzATP可抑制PD大鼠的学习记忆功能。

Optimization of High-Performance Liquid Chromatography Parameters for Purification of Oligonucleotide-A

The modification of high-performance liquid chromatography parameters leads to a more effective oligonucleotide-A purification process. Using various experimental parameters such as buffer, concentration, and pH, a method for optimizing the purification of an oligonucleotide-A on a reverse-phase C18 column was created. To purify oligonucleotide-A, High-Performance Liquid Chromatography (HPLC), Ultraviolet-Visible Spectrophotometry (UV-Vis), Liquid Chromatography-Mass Spectrometry (LC-MS), and lyophilization were used. Chromatographic data were collected with a semi-prep HPLC system, quantified with the UV-Vis technique, and validated with the LC-MS method. The most optimized parameters found to obtain the purity of 93.0% are 40 mM triethylammonium bicarbonate (TEAB) buffer with pH 7, which is approximately 6.0% higher than the reported method of which the purity is 87.0%. However, the yield under these conditions was reduced by about 5%. The worst possible optimized settings that resulted in the lowest purity (84.0%) and yield (69.0%) are 10 mM ammonium acetate (NH4CH3CO2) with pH 7.

以苄基三乙基氯化铵为增敏剂镍-溴酸钾-甲基紫体系阻抑动力学光度法测定痕量镍

在pH10.0氨水-氯化铵缓冲溶液中,镍（Ⅱ）对溴酸钾氧化甲基紫的褪色反应具有抑制性作用,阳离子表面活性剂苄基三乙基氯化铵对此体系有强烈增敏作用,据此建立了阻抑动力学光度法测定痕量镍（Ⅱ）的新方法。本法测定Ni的线性范围为0～100μg/L,检测限为8.4×10^-7g/L。该阻抑反应对甲基紫为零级反应,对溴酸钾和镍为一级反应;阻抑活化能为116.14 kJ/mol,非阻抑活化学能为78.14 kJ/mol。大部分共存离子对测定没有干扰,Cd^2＋,Cu^2＋,Co^2＋对测定有严重干扰,可预先用N530煤油萃取分离除去。方法用于铝合金和环境水样中痕量镍的测定,结果良好。

茜素红-高碘酸钾-苄基三乙基氯化铵-三乙醇胺体系催化光度法测定痕量钴(Ⅱ)

在苄基三乙基氯化铵增敏剂和三乙醇胺活化剂存在下,钴对高碘酸钾氧化茜素红的反应具有催化作用,据此建立一种测定痕量钴(Ⅱ)的新方法。考察反应的最佳条件,测定了反应动力学参数。本法在表面活性剂和活化剂存在下,其灵敏度提高9倍。线性范围为0-200μg.L-1,检出限为1.55μg.L-1。此法用于茶叶、人发等样品中钴的测定。

基于三乙胺的环氧氯丙基三乙基氯化铵的合成

采用环氧氯丙烷和三甲胺制备季铵盐型活性醚化剂环氧氯丙基三甲基氯化铵时,由于三甲胺为气态,其合成工艺较难控制,为此,探讨用液态三乙胺替代气态三甲胺合成季铵盐型阳离子醚化剂环氧氯丙基三乙基氯化铵（GTA）的方法。通过分析合成工艺参数对GTA产率的影响,获得了最佳合成工艺。并对产物GTA的元素含量、环氧值、熔点、水溶性进行了测试。GTA产率为94.53%,环氧值为90.36%,熔点在138~140℃之间。认为产品的性能优良,液态三乙胺的使用使反应过程易于操作控制,符合工业化批量生产的要求。

对甲苯磺酸三乙铵作为气相色谱固定相测定酱油中的苯甲酸

选用自行合成的对甲苯磺酸三乙铵作为气相色谱固定相，利用汞塞动态涂敷法将其制备成毛细管柱（30m×0．32mm i．d．），涂敷含量为0．125g／mL，采用外标法测定了不同产地酱油中的苯甲酸含量，分离效果好，样品回收率均在92％～102％之间，标准曲线线性良好，方法具有简便、快速、准确、重复性好等特点。

阳离子表面活性剂增敏阻抑动力学光度法测定痕量镍的研究

基于盐酸介质中,痕量镍(Ⅱ)对高碘酸钾氧化碱性中性红褪色反应的抑制作用,阳离子表面活性剂苄基三乙基氯化铵对此体系有强烈增敏作用,据此建立了表面活性剂增敏阻抑催化动力学光度法测定痕量镍的新方法,该方法测定线性范围为0～60μg/L,检出限为3.71×10-7g/L。方法用于环境水样中痕量镍(II)的测定,结果满意。

苄基三乙基氯化铵增敏阻抑动力学光度法测定食品中痕量碘

在稀硫酸介质中,阳离子表面活性剂苄基三乙基氯化铵增敏剂存在下,微量碘离子对亚硝酸根催化溴酸钾氧化维多利亚蓝的褪色反应有显著阻抑作用。据此建立表面活性剂增敏阻抑动力学光度法分析测定痕量碘的新方法。测量碘离子的线性范围为0μg/L^600μg/L,检出限为1.09×10-6μg/L。本法在表面活性剂存在下,其灵敏度提高7倍。

醋酸三乙铵离子液体中甲苯选择性氧化反应研究

以醋酸三乙铵离子液体为溶剂,硫酸亚铁为催化剂,过氧化氢为氧化剂,研究了甲苯分子中两种不同类型C—H键的选择性活化规律,优化了甲苯环C—H键优先活化的实验条件。发现在低温（40~60℃）和酸性的醋酸三乙铵离子液体（pH3~4）中反应,甲苯优先发生环羟基化反应生成甲基酚,且其深度氧化被极大抑制,获得甲基酚选择性大于60.0%,最高可达71.8%。甲苯环羟基化反应较侧链氧化反应更易受到过氧化氢浓度变化的影响,较高的过氧化氢浓度有利于环羟基化反应的进行。

新试剂溴化5,10,15-三(对甲氧基苯基)-20-丙氧苯基卟啉三乙铵与铜的显色反应

研究了新试剂溴化５，１０，１５－三（对甲氧基苯基）２０－丙氧苯基卟啉三乙铵与铜的显色反应。在ｐＨ ３～４ 的弱酸性介质中，沸水浴加热１０ ｍ ｉｎ，试剂与铜形成１∶１ 的络合物。λｍ ａｘ＝ ４１６ｎｍ ，在０～２．０ μｇ／１０ ｍ Ｌ范围内吸光度与铜的浓度关系符合比耳定律，ε＝４．９５×１０５ Ｌ·ｍ ｏｌ－ １·ｃｍ － １。该法具有灵敏度高和选择性好的特点，用于测定水样中痕量铜。

Greener approach towards the facile synthesis of 1,4-dihydropyrano[2,3-c]pyrazol-5-y1 cyanide derivatives at room temperature

This report describes triethylammonium acetate （TEAA） ionic liquid catalyzed one pot synthesis of 6-amino-4-aryl-5-cyano-3- methyl-1-phenyl-1,4-dihydropyrano [2,3-c]pyrazoles by the reaction of aromatic aldehyde, malononitrile and 3-methyl-1-phenyl-2- pyrazolin-5-one at room temperature. TEAA plays dual role as reaction media and catalyst. It can also be easily recovered and reused in several runs. TEAA provides greener reaction protocol to present methodology which obviates the need of organic solvents, expensive and toxic catalyst.

HCl溶液中酸性离子液体对Q235钢的缓蚀作用

通过电化学测试研究了N-(4-磺酸基丁基)三乙基铵硫酸氢盐([(CH2)4SO3HTEA][HSO4])酸性离子液体在25℃、0.5mol/L的HCl溶液中对Q235钢的缓蚀性能。结果表明,该离子液体在一定的浓度范围内能够减缓HCl溶液对Q235钢的腐蚀,当离子液体的浓度为14mmol/L时,缓蚀效果最好。X射线光电子能谱(XPS)表征结果表明,在Q235钢表面离子液体能够形成吸附保护膜,覆盖反应活性中心,减缓HCl溶液对Q235钢的腐蚀。

4,4’-二羟基偶氮苯合成的新方法

以对硝基苯酚为原料,在甲酸三乙胺盐和铅的作用下,在甲醇中室温反应经过还原反应得到了4,4’-二羟基偶氮苯。考察了反应时间、铅及甲酸三乙胺盐的用量对产率的影响,得出了反应的适宜条件反应时间2.5小时,铅的用量2g,甲酸三乙胺盐的用量4g,反应的转化率达82%。用红外光谱、元素分析对其进行了表征。

以苄基三乙基氯化铵为增敏剂催化光度法测定痕量铁

在增敏剂苄基三乙基氯化铵存在下，Fe（Ⅲ）对H2O2氧化溴甲酚绿具有催化作用，据此建立了一种测定痕量Fe（Ⅲ）的新方法。考察该反应的最佳条件，测定反应动力学参数。催化反应的表观活化能Ea为61．14kJ／mol。方法的检出限为2．8×10^-8g／L，线性范围0～600μg／L。用于河水、自来水等样品中铁的测定结果满意，相对标准偏差（RSD，n=6）小于5％。

甲基三乙基碳酸氢铵的合成工艺研究

甲基三乙基氢氧化铵是电子、催化等领域应用广泛的精细化工产品,可以由甲基三乙基碳酸氢铵经电解制得。以三乙胺和碳酸二甲酯为原料,采用两步法合成甲基三乙基氢氧化铵的原料甲基三乙基碳酸氢铵。从物料比、反应温度、氮气初始压力、反应时间、水解温度5个方面对合成工艺进行了优化。结果表明,在n(碳酸二甲酯)∶n(三乙胺)=1.5∶1、反应温度150℃、反应压力1.5 MPa、反应时间6 h,中间体甲基三乙基铵碳酸单甲酯的收率达90%。水解温度为70℃时,标题化合物的收率接近100%。

含离子液体乙醇-水物系等压汽液平衡数据的测定

用Ellis双循环汽液平衡釜测定了101.32kPa下乙醇-水-三乙基铵硫酸氢盐([N2,2,2,H]HSO4)的等压汽液平衡数据。实验结果表明,当[N2,2,2,H]HSO4的摩尔分数为5%时乙醇-水二组分物系的汽液平衡线就开始偏离,[N2,2,2,H]HSO4摩尔分数为10%、20%时,偏离程度增大;[N2,2,2,H]HSO4表现出盐效应,使乙醇对水的相对挥发度发生改变,消除了乙醇-水物系的共沸点;含量越大,盐效应越明显。随着[N2,2,2,H]HSO4含量的增加,乙醇对水的相对挥发度也随着增加;与其他离子液体相比较,[N2,2,2,H]HSO4具有低成本、高效率的优点,可以作为乙醇-水物系萃取精馏分离的有机盐。用NRTL模型对数据进行了关联,关联的结果和实验计算值相当,符合实验趋势。

A Novel Chromium(III) Hybrid Salt, Triethylammonium <i>Trans</i>-Diaquabis(Oxalato-<i>κ</i>²O¹,O²) Chromate(III), (C<SUB>6</SUB>H<SUB>16</SUB>N)[Cr(C<SUB>2</SUB>O<SUB>4</SUB>)<SUB>2</SUB>(H<SUB>2</SUB>O) <SUB>2</SUB>]: Synthesis, Spectroscopic Studies, Thermal Behavior and Crystal Structure

A novel organic-inorganic chromium(III) hybrid salt, triethylammonium trans-diaquabis(oxalato-κ2O1,O2)chromate(III), (C6H16N)[Cr(C2O4)2(H2O)2] (1), has been synthesized in aqueous solution and characterized by elemental and thermal analyses, FTIR and UV-Vis spectroscopies, and by single crystal X-ray structure determination. Compound 1 crystallizes in the orthorhombic system, Pbcn space group with the unit cell parameters a = 11.1776(10), b = 7.6105(10), c = 17.5654(2) Å, α = β = γ = 90°, V = 1494.24(3) Å3, Z = 4 and Z’ = 1/2. The structure of 1 consists of [Cr(C2O4)2(H2O)2]− mononuclear anions and triethylammonium [(C2H5)3NH]+ cations. In the anionic unit, the CrIII ion is six coordinated, in a distorted octahedral geometry, by four equatorial O atoms of two oxalate anions acting as chelating ligands and two O atoms from trans-coordinated water molecules occupying the apical positions with longer metal-oxygen distances. In the solid, O-H … O and N-H … O intra and inter molecular hydrogen bonding interactions connect the components into a 3D network. The triethylammonium cations are disordered among two possible orientations with occupancies rates around 50% for C4, N1, C1a, C1b, C4ii, N1ii, C1aii, C1bii (ii = −x + 1, y, − z + 1/2). The IR spectrum of 1 is consistent with the presence of the various molecular building constituents. The UV-Vis spectrum shows two absorption bands around 564 and 416 nm which are compatible with an anionic chromium (III) complex in an octahedral environment. Thermal studies carried out in air between 25°C and 700°C confirm the anhydrous character of 1 and show that it is stable up to 210°C.

取代苄基三乙基溴化铵制备与表征综合实验

取代甲苯和N-溴代丁二酰亚胺通过自由基取代反应得到取代苄溴中间体,然后用加热回流法、超声辐射法和溶剂热法3种方法,与三乙胺发生亲核取代反应,制备了5种取代苄基三乙基溴化铵,并用元素分析、红外光谱、紫外光谱、电子喷雾质谱和电导法对产物结构进行表征。该实验的取代季铵盐制备过程简单、应用广泛,涵盖常规的化学合成技术、超声波辐射制备技术、溶剂热合成技术和现代仪器分析技术和波谱解析技术等,有益于提升学生的综合技能和实践创新能力。

蔗糖八硫酸酯三乙胺梯度法制备重酒石酸长春瑞滨脂质体

目的:制备重酒石酸长春瑞滨脂质体,并对制备工艺进行考察。方法:以蔗糖八硫酸酯三乙胺(triethylammonium sucrose octasulfate,TEA8SOS)梯度法制备重酒石酸长春瑞滨脂质体,以阳离子交换树脂分离脂质体与游离药物;并以紫外分光光度法和激光粒度仪分别测定重酒石酸长春瑞滨脂质体的包封率和粒径。结果:重酒石酸长春瑞滨脂质体包封率约为95%,粒径为129.5 nm。结论:以蔗糖八硫酸酯三乙胺梯度法制备的重酒石酸长春瑞滨脂质体包封率较高,方法可行。