镱钼钒磷四元杂多化合物催化苯酚羟化分应的研究

合成了具有Keggin结构镱钼钒磷杂多化合物,用IR,UV,XRD,ICP等手段对其结构进行了表征,并研究了该杂多化合物对苯酚过氧化氢羟化反应的催化活性。实验结果表明：以甲醇为溶剂,用镱钼钒磷杂多化合物为催化剂,当（n(phOH):n(H2O2)=1:2,反应体系的pH=5.0,反应时间4h,苯酚转化率为41．66％,对苯二酚产率可达到40．24％。     

Dawson结构钼钒磷杂多化合物对苯酚过氧化氢羟化作用的研究

Ｄａｗｓｏｎ结构钼钒磷杂多化合物对苯酚过氧化氢羟化作用的研究于剑锋，杨宇，吴通好，孙家锺（吉林大学化学系理论化学研究所，长春，１３００２３）关键词Ｄａｗｓｏｎ结构钼钒磷杂多化合物，苯酚羟化，过氧化氢苯二酚（ＤＢＨ）是重要的化工原料．由芳香化合物羟化制...     

钼钒磷杂多化合物过氧化氢体系催化饱和烃的羟化反应

研究了钼钒磷杂多化合物过氧化氢体系对环己烷、正己烷和正戊烷羟化的催化性能，环己烷氧化物产率为３３．５％，醇的选择性达７３％；正戊烷氧化物产率为２３．５％，酮的选择性达７８．５％。     

Dawson结构钨钒磷杂多化合物催化苯酚过氧化氢的羟化作用及其羟化机理

合成了系列Ｄａｗｓｏｎ结构钨钒磷杂多化合物（Ｃｐｙｒ）７＋ｎＰ２Ｗ１８－ｎＶｎＯ６２（ｎ＝１～３），并用ＩＲ，ＮＭＲ等手段对其结构进行了表征．考察了这类杂多化合物对苯酚过氧化氢的羟化活性，探讨了反应机理．     

纳米磷钼钒杂多酸盐催化苯羟基化合成苯酚

纳米磷钼钒杂多酸盐催化苯羟基化合成苯酚;苯; 羟基化; 苯酚; 纳米杂多化合物     

纳米钼钒砷杂多酸盐催化苯羟化合成苯酚的研究

过氧化氢作为一种清洁氧化剂,在苯的直接羟化的研究中受到重视。催化剂主要有含钛催化剂系列、含铁催化剂系列和含铜催化剂系列、含钒催化剂系列和其它杂原子催化剂。杂多化合物是一类酸性和氧化性较强的双功能催化剂,但由于受其低比表面积的限制,导致杂多化合物固有的高催化活性在苯的过氧化氢羟化反应中难以充分发挥。本文对所制得的4种过渡金属钼钒砷杂多酸盐纳米催化剂应用于苯的过氧化氢直接羟化合成苯酚的反应,取得了苯酚收率〉50％,选择性〉98％的结果。     

Dawson结构钨钒磷杂多化合物催化苯酚过氧化氢的羟化作用及其羟化机理

合成了系列Ｄａｗｓｏｎ结构钨钒磷杂多化合物，并用ＩＲ，ＮＭＲ等手段对其结构进行了表征，考察了这类杂多化俣物对苯酚过氧化氢羟的活性，探讨了反应机理。     

镱钼钒磷四元杂多化合物催化苯酚羟化反应的研究

合成了具有Keggin结构镱钼钒磷杂多化合物 ,用IR、UV、XRD、ICP等手段对其结构进行了表征。并研究了该杂多化合物对苯酚过氧化氢羟化反应的催化活性。实验结果表明 :以甲醇为溶剂 ,用镱钼钒磷杂多化合物为催化剂 ,当n(phOH)∶n(H2 O2 ) =1∶2 ,反应体系的pH =5.0 ,反应时间 4h ,苯酚转化率为 4 1 66% ,对苯二酚产率可达到 4 0 .2 4 %。     

（CH4）15[Ce（PMo9V2O39）2].5H2O杂多配合物合成及在苯酚羟化反应中？…

合成了（ＮＨ４）１５「Ｃｅ（ＰＭｏ９Ｖ２Ｏ３９）２」．５Ｈ２Ｏ杂多化合物,并用ＩＣＰ,ＩＲ,ＵＶ,ＸＲＤ等手段对其结构进行表征,结果表明该化合物是具有Ｋｅｇｇｉｎ结构的杂多化合物。考察了该杂多化合物对苯酚过氧化氢羟化反应的催化活性,研究了反应介质、反应温度、反应时间、反应体系ＰＨ及ｍｏｌＰｈＯＨ：ｍｏｌＨ２Ｏ２对催化活性的影响。实验结果表明：以甲醇为溶剂,用标题化合物作催化剂,当ｍｏｌＰｈＯＨ：ｍ     

三取代钨硅杂多配合物的磁性

三取代钨硅杂多配合物的磁性＊王力刘宗瑞周云山王恩波＊＊（东北师范大学化学系长春１３００２４）关键词钨硅杂多化合物磁性Ｊｇ中图分类号Ｏ６４１．４杂多化合物具有独特的结构，因此具有许多优异性能，尤其是混配取代型杂多化合物［１］，具有优异的热稳定性、氧化还...     

Pyridine-keggin heteropoly compounds as catalyst for hydroxylation of phenol using hydrogen peroxide as oxidant

The pyridine-heteropoly compounds are very active catalysts for phenol hydroxylation to dihydroxybenzenes with hydrogen peroxide as oxidant in aqueous solutions. The conversion of phenol reaches 77.8%, and the selectivity for dihydroxybenzenes reaches 99%.     

Study of the behaviour of various phenolic compounds in the 4-aminoantipyrine and ultraviolet-ratio spectrophotometric methods without and with distillation

It is customary in industrial analysis in the determination of phenols by the 4-aminoantipyrine (4-AAP) and ultraviolet-ratio spectrophotometric methods to report the total of phenolic compounds as phenol. A study was therefore made of the behaviour of 36 representative phenolic compounds in the 4-AAP and UV-ratio methods, with and without distillation, to ascertain the apparent recoveries relative to that for phenol. The Fisher phenol analyser was used for the UV-ratio method, which depends upon the bathochromic shift (from about 270 to about 290 nm) usually obtained when the solution of the phenol is made alkaline. The apparent recoveries by the 4-AAP method both with and without distillation varied from 0 to 100%. The apparent recoveries by the UV-ratio method without distillation varied from 0 to 148%, and those with distillation varied from 0 to 110%. Sixteen of the compounds tested without distillation gave less than 10% recovery by the 4-AAP method and eleven gave less than 10% recovery by the UV-ratio method. The results after distillation indicated that several of the compounds did not distil completely.     

A WATER-COMPATIBLE PHENOLIC HYDROXYL MODIFIED POLYSTYRENE AS AN ADSORBENT FOR ADSORBING PHENOLIC COMPOUNDS FROM AQUEOUS SOLUTIONS

1. INTRUDUCTION As most phenolic compounds are extremely toxic at the concentrations discharged into accepting effluents, the removal or destruction of phenolic compounds from such streams has become a significant environmental task [1]. Increasing concern for public health and environmental quality has led to the establishment of limits on the acceptable environmental levels of specific pollutants [2]. Consequently there has been a growing interest in developing and implementing various …     

A WATER-COMPATIBLE PHENOLIC HYDROXYL MODIFIED POLYSTYRENE AS AN ADSORBENT FOR ADSORBING PHENOLIC COMPOUNDS FROM AQUEOUS SOLUTIONS

A water-compatible phenolic hydroxyl modified polystyrene adsorbent (AM-1) foradsorbing and removing phenolic compounds from aqueous solutions was prepared by covalent bonding of phenolic hydroxyl groups to the surface of porous polystyrene-divinylbenzene beads, this resin can be used directly without wetting process. A comparison of the sorption properties of the new resin and Amberlite XAD-4 toward four phenolic compounds, phenol, p-cresol, p-chlorophenol,and p-nitrophenol was made. The capacities of equilibrium adsorption of AM-l for all four phenolic compounds increased around 20% over that of Amberlite XAD-4, which may be contributed to phenol hydroxyl group on the surface and the unusual pore distributior. At their dilute solution, the equilibrium adsorption capacities of AM-1 for phenol increased about 62% over that of Amberlite X4D-4, while equilibrium adsorption capacities of the other three phenolic compounds increased 4-35%, suggesting an advantage of AM-I over Amberlite XAD-4 in the collection of phenol.Freundlich isotherm equations and isosteric adsorption enthalpies for the four phenolic compounds indicate a physical adsorption process on the Amberlite XAD-4 and AM-I resins. Column studies for phenol show that AM-1 resin has excellent adsorption and desorption performance.     

A WATER—COMPATIBLE PHENOLIC HYDROXYL ODIFIED POLYSTYRENE AS AN ADSORBENT FOR ADSORBING PHENOLIC COMPOUNDS FROM AQUEOUS SOLUTIONS

A water-compatible phenolic hydroxyl modified polystyrene adsorbent (AM-1) for adsorbing and removing phenolic compounds from aqueous solutions was prepared by covalent bonding of phenolic hydroxyl groups to the surface of porous polystyrene-divinylbenzene beads,this resin can be used directly without wetting process.A comparison of the sorption properites of the new resin and Amberlite XAD-4 toward four phenolic compounds,phenol,p-cresol,p-chlorophenol,and p-nitrophenol was made.The capacities of equilibrium adsorption of AM-1 for all four phenolic compounds increased around 20% over that of Amberlite XAD-4,which may be contributed to pheonl hydroxyl group on the surface and the unusual poe distribution.At their dilute solution,the equilibrium adsorption capacities of AM-1 for phenol increased aout 62% over that of Amberlite XAD-4,while equilibrium adsorption capacities of the other three phenolic compounds increased 4-35%,suggesting an advantage of AM-1 over Amberlite XAD-4 in the collection of phenol.Freundlich isotherm equations and isosteric adsorption enthalpies for the four phenolic compunds indicate a physical adsorption process on the Amberlite XAD-4 and AM-1 resins,Column studies for phenol show that AM-1 resin has excellent adsorption and desorption performance.     

Highly stable electrochemical oxidation of phenolic compounds at carbon ionic liquid electrode

A carbon ionic liquid electrode (CILE) was used for the investigation of the electrochemical oxidation of phenolic compounds in acidic media using cyclic voltammetry, chronoamperometry and square wave voltammetry techniques. The results indicate that, contrary to many other electrodes, the oxidation of phenolic compounds on CILE is highly stable and does not result in electrode fouling. Cyclic voltammetry showed that phenolic compounds such as phenol, 2,4-dichlorophenol and catechol were oxidized at CILE and remained electroactive after multiple cycles and at high concentrations of phenol. The cyclic voltammetric response of the CILE is very stable with more than 99% of the initial activity remaining after 20 s of stirring of a 0.5 mM solution of phenol.     

一种亲水的酚羟基修饰聚苯乙烯树脂对酚类化合物的吸附热力学

在283-323K和研究的浓度范围内,苯酚、对甲苯酚、对氯苯酚和对硝基苯酚在亲水性的酚羟基修饰聚苯乙烯树脂（AM-1）与大孔吸附树脂（Amberlite XAD-4)上平衡吸附数据符合Freundlich吸附等温方程。酚类化合物在AM-1上的吸附容量比在Amberlite XAD-4上的吸附容量增加20%以上,这主要得益于AM-1表面的酚羟基入树脂的微孔结构。在较稀的溶液中AM-1对苯酚的吸附量比AmberliteXAD-4对苯酚的吸附量增加60%,表明AM-1对苯酚有特殊的选择性。Freundlich吸附等温线、相对吸附容量以及等量吸附焓表明,四种酚在两种树脂上的吸附是物理吸附过程。对酚类化合物被两种树脂吸附的吸附焓、自由能、吸附熵也作了测试,并对吸附行为作了合理的解释。     

固相萃取-微乳液相色谱法测定环境水体中的3种酚类化合物

建立了固相萃取-微乳液相色谱法同时测定环境水体中的苯酚、双酚A (BPA)、2,4-二氯苯酚3种酚类化合物的检测方法。水样加酸酸化后,经C18固相萃取小柱富集净化,用微乳液相色谱法测定3种目标物的含量。在Inertsil C18色谱柱(150 mm×4.6 mm, 5 μm)上以微乳(3.0%十二烷基硫酸钠(SDS)-6.0%正丁醇-0.8%正庚烷-90.2%(水+0.5%HAc))和乙腈作为流动相进行梯度洗脱,流速1.0 mL/min,检测波长280 nm。结果表明,苯酚、双酚A、2,4-二氯苯酚的检出限(S/N=3)依次为0.74、8.0、8.0 μg/L,线性范围在0.1~10 mg/L范围内,相关系数(r)均大于0.999。将3种酚类化合物定量加到空白水样中,苯酚、双酚A、2,4-二氯苯酚的加标回收率分别为82.7%、87.8%、82.6%,其RSD均小于5%(n=6)。对环境水样的酚类化合物分析也取得了良好的加标回收率,其值均在85.7%~113.2%之间。结果表明,该方法准确可靠、灵敏度高,适用于环境水体中酚类化合物的检测。     

New hydrophilic polymeric resin based on 4-vinylpyridine-divinylbenzene for solid-phase extraction of polar compounds from water

A 4-vinylpyridine-divinylbenzene (VP-DVB) resin was synthesized to be used for on-line solid-phase extraction process and it was tested for a group of polar compounds. The high specific surface area and the nitrogen content of the VP-DVB sorbent increased the interactions with the polar analytes in the preconcentration process. The sorbent enabled 100 ml of water to be concentrated with recoveries higher than 70% for several polar compounds (including phenol) except for oxamyl (55%) and methomyl (43%). The method was used to analyse water samples by liquid chromatography and UV detection. Linearity was good and detection limits were 0.1-0.2 microg l(-1) for all compounds. Several tap and river water and waste water treatment plant samples were analyzed; phenol and (4-chloro-2-methyl-phenoxy)acetic acid (MCPA) were tentatively determined in some samples.     

Tenax采样管富集气相色谱-质谱法测定空气中的痕量酚类化合物

建立了Tenax采样管富集气相色谱-质谱测定空气中痕量酚类化合物的方法。用Tenax采样管吸附环境空气中的痕量酚类化合物,用甲醇淋洗解吸酚类化合物,洗脱液加入萘-D8作为内标,利用气相色谱-选择离子监测质谱(GC-MS/SIM)进行检测,内标法定量。该方法定性、定量准确,线性响应良好,回归曲线的线性相关系数均大于0.999,平均回收率为92.4%～102%,测定干扰小,检测灵敏度高,按采样10 L计算,空气中最低检测浓度可达0.001 mg/m3。用于实际样品测定,完全能满足环境空气中痕量酚类化合物监测的要求。