溴胺酸Ullmann缩合反应工艺

采用强酸阳离子交换树脂-乙醇-铜粉催化体系代替传统工艺中硫酸-水-铜粉催化体系,对溴胺酸进行Ullmann缩合反应。考察了强酸离子交换树脂用量、有机溶剂种类及反应温度等因素对反应收率的影响。结果表明,在V(乙醇)∶V(水)=9∶1介质中,在溴胺酸、铜粉存在下,树脂用量为16g/L,在70℃下反应3h,溴胺酸缩合产物收率可达94.0%。反应中所使用的离子交换树脂、铜粉和乙醇均可回收再利用,强酸离子交换树脂重复使用5次后其催化活性仍未降低;乙醇回收率可达70%～80%,铜粉的回收率可达85%～90%。     

高效液相色谱法检测化妆品中着色剂罗丹明B、金光红C和颜料红57

采用N,N-二甲基甲酰胺提取样品中的待测物,建立了化妆品中禁、限用着色剂罗丹明B、颜料红57和金光红c的高效液相色谱检测方法。以XDB-C18柱为分析柱,5mmol／L四丁基氢氧化铵-氢氧化钾水溶液（磷酸调至pH7．00）和甲醇为流动相,梯度洗脱。550am（罗丹明B）和480nm（颜料红57和金光红C）为检测波长,柱温30℃,流速1．0mL／min,保留时间定性,外标法定量。结果表明在0．25-20mg／L（罗丹明B和金光红C）、0．5-40mg／L（颜料红57）浓度范围内线性关系良好,检出限分别为5,20,20mg／kg（S／N=10）,实际样品中的加标回收率分别为94．8％～100．5％,95．1％～103．1％,82．5％-90．5％,相对标准偏差为0．9％～4．6％。该方法前处理简单、易操作,检测结果准确可靠。能够满足化妆品中这3种着色剂的检测要求和监管需要。     

高压微波制备Pt／C催化剂的工艺研究

利用高压微波消解仪密闭带压、升温速率可控的特点,选择XC-72碳黑为载体,乙二醇为碳黑分散溶剂和还原剂,研究反应温度、升温速率、水含量、Pt含量及表面活性剂等工艺条件对Pt粒子尺寸及其分散度的影响．研究结果表明,快速升温到190℃、控制反应体系中水含量和Pt含量等工艺条件,可以得到Pt粒子平均粒径小于3．1nm的Pt／C催化剂,且Pt粒子分布均匀,无团聚．     

苏丹红I分子印迹聚合物的制备及其性能评价

以苏丹红I为模板分子,通过沉淀聚合法制备了一种对苏丹红I具有特异性吸附的分子印迹聚合物。通过选择性评价和前沿色谱实验,评价了致孔剂的选择和用量、功能单体和模板分子的物质的量比对分子印迹聚合物识别性能的影响。实验结果表明: 当以甲醇和乙腈的混合液(体积比为30:10)为致孔剂,甲基丙烯酸(MAA)为功能单体,且功能单体和模板分子的物质的量比为8:1时,分子印迹聚合物的印迹因子为2.32,亲和位点总数(Bt)为0.50 μmol/g;将其作为固相萃取柱填料用于辣椒粉样品中痕量苏丹红I的净化和富集,结果表明: 苏丹红I浓度在10～500 μmol/L范围内时,呈现良好的线性关系(r=0.999);检出限为3.3 μmol/L,加标回收率为95.87%～98.41%,相对标准偏差低于3.1%。该方法有望用于辣椒粉样品中苏丹红I添加剂的常规检测。     

丙烯酸酯共聚物对红颜料PR48:2的分散作用

丙烯酸酯共聚物对红颜料PR48:2的分散作用     

C.I.颜料红31的亲水化改性及其在水性油墨中的应用性能研究

为提升C.I.颜料红31的亲水性,使之更加适用于水性油墨,在颜料生产的偶合过程中选用2-羟基-3-萘甲酰基-(4′-氯-2′,5′-双甲氧基)苯胺(色酚AS-LC)参与2-羟基-3-萘甲酰基间硝基苯胺(色酚AS-BS)偶合剂的制备,并与3-氨基-4-甲氧基-苯甲酰苯胺(红色基KD)的重氮产物进行偶合反应,制得水性C.I.颜料红31。接触角、SEM、色光、热重分析结果表明,经过色酚AS-LC改性的颜料样品晶体形貌可由长条状转呈圆片状,其用量为5%(mol)时,可使颜料与水之间的接触角降至53.4°,粒径及粒径分布明显变窄,具有最佳的亲水性能。色酚AS-LC与色酚AS-BS的共偶合会使颜料色样偏向红色和蓝色,但色差(ΔE)较小,值为0.52。氮气氛中加热至270℃颜料晶体开始分解,达到了耐高温颜料的标准。制备成水性油墨并测试其易分散性、流变性能及相关印刷适性,结果显示均明显优于未经水性化改性的C.I.颜料红31。     

Didemnaketal A类似物的合成研究──C8-C15中间体的合成

DidemnaketalA是一类具有明显抗艾滋病活性的天然螺环缩酮类化合物^[1],但至今未见有关合成及立体化学研究的报道.为进一步研究这类螺环缩酮类化合物的生理活性,我们开展了侧链简化的类似物(如化合物1)的合成研究.     

Didemnaketal A类似物的合成研究──C1-C7中间体的合成

寻找抗艾滋病活性的抚导化合物是当前药物化学研究领域中的热点之一.     

直接甲醇燃料电池阳极催化剂PtRu/C的制备和表征

用三种方法制备了PtRu/C[Pt和Ru质量分数分别为20％和10％,记为PtRu/C(20％-10％)]甲醇阳极催化剂,通过X射线衍射(XRD)和透射电镜(TEM)考察了PtRu/C催化剂的粒子大小和晶格参数的变化,利用单电池实验考察了催化剂在直接甲醇燃料电池中的催化活性.结果表明,改变溶剂的组成提高了贵金属在活性炭表面的分散度,并改善了PtRu间的相互作用,用乙二醇/水/异丙醇混合溶剂制备的PtRu催化剂金属颗粒较小,PtRu间的相互作用较强,以该催化剂作甲醇阳极的直接甲醇燃料电池的性能较好.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定工业废水中的颜料绿58

建立了硝酸溶解-电感耦合等离子体原子发射光谱(ICP-AES)法测定工业废水中颜料绿58的分析方法。方法前处理简单,在选定的条件下,检出限为3.0×10-3 mg/L,方法的相对标准偏差小于3%,样品加标回收率在95.0%~105%。方法准确,快速,可用于水中颜料绿58的定量分析。     

水滑石焙烧产物对弱酸艳红B吸附特性研究

以Mg(NO3)2·6H2O和AL(NO3)3 - 9H2O为原料,NaOH、NaCO溶液作混合沉淀剂,采用水热法可制得结晶度很高的、具有规整的层状结构水滑石.水滑石经500℃焙烧可使其结构完全被破坏得对应的焙烧产物,该焙烧产物对弱酸艳红B染料有很强的吸附能力.在200 mL 100 mg/L弱酸艳红B溶液中,加入40...     

Kinetics and products of ozonation of C.I. Reactive Red 195 in a semi-batch reactor

Textile wastewater shows great threats to the environment if not well pretreated before discharge. A promising technique, ozonation, was applied to remove the color in dye solutions containing C.I. Reactive Red 195 (RR195) in a semi-batch reactor. The decolorization of RR195 by the ozone process followed pseudo-first-order kinetics. Several factors which influenced the efficiency of decolorization were studied and the reaction rate constant (k) obtained with different operational parameters was compared. Our results showed that RR195 was more easily degraded in acidic than in alkaline conditions. The dyeing auxiliaries (sodium carbonate and sodium chloride) that acted as radical scavengers could enhance the decolorization process, and the ozonation time for total color removal lengthened if the initial dye concentration was higher. The analysis of the ozonation products was performed by liquid chromatography-tandem mass spectrometer and a possible degradation pathway was predicted according to the ozonation products and structure of RR195. Our results indicated that ozonation was effective in the color removal of dyes, but further treatment might be necessary since the ozonation products are high toxic.     

Preparation of Pt／C Catalyst with Solid Phase Reaction Method

The Pt/C catalyst was prepared with solid phase reaction method (Pt/C(S)) for the first time.Its Performances were compared with that prepared by the traditional liquid phase reaction method. The results demonstrate that the electrocatalytic activity of Pt/C catalyst with solid phase reaction method for methanol oxidation is higher than that with liquid phase reaction method. XRD and TEM measurements indicate that the Pt/C(S) possesses low crystalline extent and small particle size.     

Preparation of Pt／C Catalyst with a New and Simple Organic Sol Method

It is reported for the first time that the Pt/C catalyst can be prepared with a new and simple organic sol method using SnCl2 as the reductant. It was found that the average size of the Pt particles in the Pt/C catalysts could be controlled with controlling the preparation conditions. The effect of the average sizes of the Pt particles in the Pt/C catalysts obtained with this method on the electrocatalytical activity of the oxidation of methanol was investigated.     

An Efficient Nanoparticle‐Supported and Magnetically Recoverable Copper(I) Catalyst for Synthesis of Furans from Ene‐yne‐ketone

A magnetic nano‐supported Cu(I) catalyst was prepared and showed high activity for cyclization of ene‐yne‐ketone to synthesize furans. The catalyst was easily recovered from the reaction by using external magnets and reused 8 times without significant loss of its catalytic activity.     

Studies of C. I. Acid Red 186 and Metal Complexes with Uo++2, Ce3+ and Th6+ Ions

The electronic absorption spectra of C. I. Acid Red 186 are studied in solution of different pH. The pK values of the acid-base equilibria set are determined and commented upon. The complexes of UO⁺⁺₂, Ce³⁺ and Th⁴⁺ ions are investigated by some spectroscopic techniques and potentiometric titration. The formation of 1:1, 1:2 and 1:2 complexes (M:L) with UO₂⁺⁺, Ce³⁺ and Th⁴⁺ respectively is confirmed and their conditional stability constants are determined. The solid complexes are prepared and analysed for their metal content, their ir spectra are disussed in comparison to that of the ligand to establish the bonding between the ligand and metal ions.     

An Efficient Method for the Preparation of Sulfonamides from Sodium Sulfinates and Amines

Sulfonamides have a special role on medicine due to their broad biological activities, as bacterial infections, diabetes mellitus, oedema, hypertension prevention and treatment. In addition, sulfonamides are also useful in herbicides and pesticides. Herein, we communicate an efficient strategy for the preparation of sulfonamides via NH₄I‐mediated amination of sodium sulfinates. This new method provides a general and environmentally friendly access to sulfonamide compounds and tolerates a wide range of functional groups.     

Sonocatalytic degradation of C.I. Reactive Red 198 in H2O2-based Systems

This study elucidated the effects of pH on the decolorization of C.I. Reactive Red 198 (RR198) in US, UV/H₂O₂, US/H₂O₂ and UV/US/H₂O₂ systems. The synergistic effects in US/H₂O₂ and UV/US/H₂O₂ systems were also evaluated. At pH 4, 7 and 10, the decolorization rates of RR198 followed the order UV/US/H₂O₂ > UV/H₂O₂ > US > US/H₂O₂.