无致癌诱变性二元胺的直接染料

综述了用2,2'-二甲基-5,5'-二丙氧基联苯胺和5,5’-二丙氧基联苯胺作为重氮组分的直接染料的合成和检测。TLC检测染料的纯度,其最大可见吸收为485-601nm,摩尔消光系数为2.2×104-6.4×104L/mol.cm,用ESMS确定染料的化学结构。这类直接染料无致癌诱变性,并具有良好的应用和牢度性能。有20篇参考文献。     

2-氯-4,6-二硝基间苯二酚的结晶动力学研究

采用间歇动态法测定了2-氯-4,6-二硝基间苯二酚(CDNR)的结晶动力学参数,并回归了CDNR的结晶动力学方程,分析了结晶动力学的影响因素。通过回归结晶成核速率方程和生长速率方程的计算,得到了一定温度、一定搅拌速度下的成核、生长速率常数,温度27℃、搅拌速度180 r.min-1时成核速率常数和成长速率常数分别为9.17×106和2.17×10-12,温度33℃、搅拌速度240 r.min-1时成核速率常数和成长速率常数分别为2.02×108和7.10×10-12。     

防晒剂2,4-二羟基二苯甲酮的极谱行为研究

用线性扫描极谱法研究了2,4-二羟基二苯甲酮分别在B-R缓冲溶液中的极谱行为。实验表明,在pH4.30的B-R缓冲溶液中,2,4-二羟基二苯甲酮的二阶导数峰电位为-1.20V(vs.SCE),二阶导数峰电流与其浓度在5.0×10-7mol.L-1~8.0×10-6mol.L-1内有良好线性关系,线性方程为ip″(nA.s-2)=45.48+1.034×108c(mol.L-1),线性相关系数为0.9999,为不可逆吸附波。     

二甘醇的综合利用技术新进展

二甘醇（DEG）是环氧乙烷用水合法生产乙二酵（EG）的副产物,随着我国乙二醇工业的迅速发展二甘醇产量不断增加,充分利用二甘醇资源开发下游产品、拓展二甘醇的用途越来越受到重视。综述了国内二甘醇的综合利用进展,介绍了二甘醇的直接利用途径和二甘醇合成吗啉、二甘醇醚、二甘醇酯、1,4-二氧六环、二甘酸和二甘醇胺等精细化学品的利用情况。     

二醋酸纤维素的X—射线衍射初探

本文将二醋酸纤维素溶于丙酮使其重结晶,利用X—射线衍射方法,研究了二醋酸纤维素的晶胞参数,实验结果表明,二醋酸纤维素为正交晶系,a=24.5×10~(-10)m,b=11.6×10~(-10)m,c=10.43×10~(-10)m。     

利用四氮杂大环镍配合物催化Briggs-Rauscher振荡反应测定2,6-二叔丁基4-甲基苯酚的新方法

报道了一种利用四氮杂大环配合物催化Briggs-Rauscher(BR)振荡反应测定2,6-二叔丁基-4-甲基苯酚(BHT)的方法,所涉及的体系为H2SO4-KIO3-[NiL](ClO4)2-MA-H2O2(其中L为四氮杂大环5,7,7,12,14,14-六甲基-1,4,8,11-四氮环杂十四4,11-二烯,MA表示丙二酸).通过研究发现,在该体系中加入一定浓度的BHT,会使得振荡体系的周期、振幅等都发生改变,同时体系会产生抑制时间.当BHT浓度在1.95×10-7 ～6.25×10-6 mol/L范围内,抑制时间与加入的BHT浓度呈很好的二次函数关系;当BHT浓度在6.25×10-6 ～ 1.56×10-5 mol/L范围内,抑制时间与加入的BHT浓度呈很好的一次线性关系.为了达到更好的定量检测效果,对各组分的浓度进行了优化,使得检测效果达到最佳,最后对反应机理进行了探讨.     

气相色谱-质谱联用法对3-氯亚氨基二苄中杂质的研究

应用气相色谱-质谱联用方法研究3-氯亚氨基二苄中的杂质。在30.0m×0.25mm,0.5μm的ZB-5MS毛细管柱上,柱温100°C保持3min,后以20°C/min的速率程序升温至250°C,气化室温度270°C,载气氦气流量0.8mL/min的条件下,3-氯亚氨基二苄及其中杂质获得很好分离。通过对各组分质谱图分析,并结合反应过程确定了3-氯亚氨基二苄中的四种杂质分别为亚氨基二苄,甲基亚氨基二苄酮,10-氯-5H-二苯并[b,f]氮杂和3,7-二氯-10,11-二氢-二苯并[b,f]氮杂。     

[Pb(DNI)_2(H_2O)_4]的制备和晶体结构

通过2,4-二硝基咪唑(2,4-DNI)的钠盐水溶液与硝酸铅的水溶液反应,制备出了2,4-二硝基咪唑铅配合物;采用自然挥发法培养出了适于X光结构测定的单晶,X射线衍射测定结果为,晶体属单斜晶系,空间群为Cc,晶体学参数为:a=6.517(3)×10-1nm,b=17.131(6)×10-1nm,c=14.082(7)×10-1nm,α=90.00(3)°,β=97.80(4)°,γ=90.00(4)°,V=1 557.5(12)×10-3nm3,Z=4,Dc=2.531 g/cm3,μ=11.001 mm-1,F(000)=1 120,最后偏离因子R为0.022 6。根据红外光谱、元素分析和X射线衍射分析结果,确定了2,4-二硝基咪唑铅配合物的化学组成为C6H10O12N8Pb,分子结构式为[Pb(DNI)2(H2O)4]。     

2-苯基-4-对氯苯基-1,5-苯并硫氮杂-α-(丁二酰亚胺基)-β-内酰胺的高效液相色谱法分析

采用Hypersil-ODS2(4.6mm×250mm,5μm)色谱柱,乙腈-水(70∶30)流动相,242nm检测波长,建立了测定2-苯基-4-对氯苯基-1,5-苯并硫氮杂-α-(丁二酰亚胺基)-β-内酰胺的高效液相色谱法。该法线性范为0～0.1mg/mL,回归方程为A=1.63×108c-2.86×105,相关系数r=0.9994,相对标准偏差为0.33%(c=0.06mg/mL,n=5),检出限为0.08μg/mL。平均回收率在97.2%～102.4%之间。该法重现性好,灵敏度高,简单,快速,准确。     

一种含有推-拉电子基团的水溶性大π共轭高分子的合成与表征

通过5步法合成了一种含推-拉电子基团、窄能隙(Eg=1 63～1 87eV)、大π共轭高分子———聚[(3 乙酰基吡咯) 2,5 二(对二甲氨基苯甲烯)](PAPDMABE)。该聚合物能溶于多种极性有机溶剂和酸性水溶液,在c(HCl)=0 5mol/L的水溶液中溶解度为0 72～0 81g/mL。采用氢核磁谱、傅里叶红外光谱、紫外-可见光谱、分光光度计等分析手段对反应中间产物、聚合物PAPDMABE及其前聚物聚[(3 乙酰基吡咯) 2,5 二(对二甲氨基苯甲烷)](PAPDMABA)进行了分析。通过碘掺杂和w(H2SO4)=98%的浓硫酸掺杂处理,PAPDMABE的电导率提高了3～4个数量级,分别为1 2×10-6S/cm和4 3×10-5S/cm。     

Upper and lower critical solution temperatures in poly (ethylene glycol) solutions

Upper and lower critical solution temperatures have been determined for solutions of poly(ethylene glycol) in t-butyl acetate and water over the molecular weight range of M_η = 2.18 × 10³ to ～1020 × 10³. The phase diagram for solutions of poly(ethylene glycol) (M_η = 719 × 10³) in t-butyl acetate was expressed as the ‘hour glass’ type, while the phase diagram for solution of poly(ethylene glycol) (M_η = 2.18 × 10³ to ～2.29 × 10³) in water was expressed as the ‘closed loop’ type. The value of the pressure dependence of the lower critical solution temperature $\text{(}\text{d}\text{T}\text{d}\text{P}\text{)}{}_{\mathrm{c}}$ in the poly(ethylene glycol) (M_η = 1020 × 10³)/water system over the pressure range of 0 to ～50 atm was negligibly small and positive.     

Tetrahydrofuran polymerization initiated by heteropolyacid in the presence of ethylene oxide: Reaction behavior of water and glycol

The reaction behavior of water and low molecular weight glycol in tetrahydrofuran polymerization initiated by H₃PW₁₂O₄₀ in the presence of ethylene oxide has been studied. A lot of water was used in the hydrolysis reaction of ethylene oxide at the early stage of the polymerization and transformed into ethylene glycol (EG), which was consumed subsequently through a chain transfer reaction. EG was more reactive both than 1,4‐butylene glycol and hexamethylene glycol toward propagating species, and the reaction rate constants at 0°C were determined by GC to be 0.142, 8.83 × 10⁻², and 5.53 × 10⁻² L · mol⁻¹s⁻¹, respectively. The molecular weight of the product can be predicted by an equation based upon conversion of polymerization and the concentrations of molecular weight controller and H₃PW₁₂O₄₀. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 1821–1826, 1999     

双磷酸酯表面活性剂的合成与性能

以三氯氧磷、二元醇(酚)、正十二醇为原料,合成了4种双十二烷基双磷酸酯(HDP,DGDP,BDP,PDP)。产物经无水乙醇重结晶提纯后,通过IR、1HNMR、质谱和电位滴定进行了结构表征。25℃时,它们的电离常数分别为:2.76×10-5mol/L(HDP),3.940×10-4mol/L(DGDP),1.595×10-4mol/L(BDP),4.255×10-3mol/L(PDP)。20℃时,它们的临界胶束浓度分别为:3.5×10-4mol/L(HDP),9.0×10-4mol/L(DGDP),1.1×10-3mol/L(BDP),1.3×10-3mol/L(PDP);在临界胶束浓度处的表面张力分别为:30.38 mN/m(HDP),34.49 mN/m(DGDP),35.31 mN/m(BDP),36.14 mN/m(PDP)。差热分析表明,4种产物的分解温度分别为:231℃(BDP),251℃(HDP),227℃(PDP),249℃(DGDP);初熔温度分别为:87℃(BDP),80℃(HDP),97℃(PDP),72℃(DGDP)。     

Effective promotion of tetrahydrofuran polymerization initiated with heteropolyacid

Tetrahydrofuran was polymerized using the heteropolyacid H₃PW₁₂O₄₀ as the initiator and ethylene oxide as the promoter, which effectively increased the rate and conversion of the polymerization. Water and butylene glycol were used to control the molecular weight of the product in the range of 1000–3000. The polymer was found to be polyether glycol containing 10–22 mol % oxyethylene moieties with hydroxyl groups at both chain ends. The melting point was ∼ 10°C lower compared to polytetramethylene ether glycol having the same molecular weight. The concentration of active species remained unchanged in the main period of the polymerization, indicating the absence of chain termination. The values of the chain propagation rate constant of tetrahydrofuran polymerization at 0 and 20°C were found to be 3.78 × 10⁻³ and 1.98 × 10⁻² L mol⁻¹ s⁻¹, respectively, which are close to the rate constant of chain propagation of tetrahydrofuran on ionic active species. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 2303–2308, 1999     

马来酸乙二醇酯、丙烯酸共聚物合成与在水质稳定上的应用研究

合成了马来酸与乙二醇的酯化物。用该酯化物与丙烯酸二元共聚，及用该酯化物、丙烯酸、马来酸酐三元共聚，得到了两种共聚物。讨论了二元共聚物的特性粘数与单体用量的关系，并测定了二元共聚物及三元共聚物对Ｃａ２＋的螯合能力。     

衣康酸单酯羧酸盐Bola表面活性剂性能

以衣康酸酐(IAn)和聚丙二醇400 (PPG 400)为原料,经过酯化反应和酸碱中和反应制备出衣康酸基聚丙二醇单酯羧酸盐Bola型表面活性剂(Saa-K)。利用1H NMR、FT IR对其结构进行了表征。对Saa-K的表面张力、临界胶束浓度(CMC)、润湿性、泡沫性能等进行了测试,考察了电解质对Saa-K溶液的表面张力和CMC的影响。结果表明：常温常压下,Saa-K的表面张力为32.46 mN/m、临界胶束浓度为1.715×10-2 mol/L;当溶液中Saa-K的质量分数为1%时,Saa-K的第一临界相变温度TK1＜0 ℃;第二临界相变温度TK2为54.3 ℃;当溶液中Saa-K和月桂酸钾(PL)的质量分数均为1%时,Saa-K的起泡高度和泡沫寿命分别为51.13 mL和1940 min,而月桂酸钾的起泡高度和泡沫寿命分别为98.53 mL和2200 min。在阴离子强度相同或阳离子强度相同的情况下,无机电解质的加入均会使Saa-K溶液的表面张力和CMC显著降低,降低程度分别为：LiCl＜NaCl＜KCl和NaBr＜NaCl＜NaF。     

甲苯-苯甲醛-苯甲酸体系汽液平衡的研究

本文在600×1.333×10~2Pa和400×1.333×10~2Pa压力下分别测定了甲苯-苯甲醛-苯甲酸三元体系及其三个二元体系的汽液平衡数据。用点检验法对二元数据进行了热力学一致性检验,并用Margules、wilson、NRTL和UNIQUAC方程作热力学关联。预测了三元汽液平衡关系,与实测值吻合结果令人满意。     

Influences of nonionic poly(ethylene glycol) polymer PEG on electrokinetic and rheological properties of bentonite suspensions

The determination of the electrokinetic properties of colloidal systems is very important for the chracterization of these systems. Colloidal systems have high adsorption performance due to the carrying of negative charges and the colloid structure. The control of the electrokinetic properties of the bentonite–water system are important not only from a technological point view; they are also important from a scientific point of view. Knowing the electrokinetic and rheological properties of bentonite minerals is important for the estimation of the behavior of clays under various environmental conditions. The purpose of this study was to interpret the effect of the nonionic poly(ethylene glycol) (PEG) polymer on electrokinetic and rheological properties. Zeta potential and viscosity measurements were done as a function of PEG molecular weights (400, 3000, and 8000) and their concentrations (2.5 × 10^?5 to 1.25 × 10^?2 mol/L). We interpreted the experimental data, taking into account these two parameters. X‐ray diffaction studies were done together with the electrokinetic and rheological measurements. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 341–346, 2002     

Two Nanostructured Polymers: Polyaniline Nanofibers and New Linear-dendritic Matrix of Poly(citric acid)-block-poly(ethylene glycol) Copolymers for Environmental Monitoring in Novel Biosensors

In this work two phenol biosensors, one based on polyaniline nanofibers (PNFs) and the other based on the newly created and introduced linear-dendritic matrix of poly(citric acid)-block-poly(ethylene glycol) copolymers (PCA-PEG-PCA), were chemically modified with horseradish peroxidase (HRP) enzyme. These phenol biosensors showed an oxidation peak at 0.55 V. The amperometric response for biosensors based on PNFs showed a linear response range from 2.5 × 10^?6 to 2.5 × 10^?5 mol/L, with a detection limit of 2.5 µM phenol. Also, the amperometric response for a biosensor based on PCA-PEG-PCA showed a linear response range from 2.5 × 10^?6 to 4 × 10^?5 mol/L, with a detection limit of 1.5 µM phenol.     

Electrical performance of lithium ion based polymer electrolyte with polyethylene glycol and polyvinyl alcohol network

A solid polymer electrolyte based on lithium hydroxide (LiOH) added with polyethylene glycol and polyvinyl alcohol polymers was synthesized by solution casting. The structural variation with respect to loading wt% of LiOH reveals the semicrystalline property of polymer electrolyte. The differential scanning calorimetry data shows the onset of crystalline to amorphous transition, which occurs nearly to the melting peak, for higher salt content. The structural properties and cross-linking between polymer and salt were demonstrated by polarized optical microscopy. The polymer electrolytes were subjected to AC impedance analysis spectra for obtaining the ionic conductivity at different temperature. The charge carriers relax much faster for higher lithium salt concentration based polymer electrolyte and produces higher conductivity. The highest room temperature conductivity 2.63 × 10^?5 S/cm is obtained for 8 wt% loading of lithium salt based polymer electrolyte, confirming their use in preparation of ion conducting devices.