Preparation of silica supported 1-nitroso-2-naphthol-grafted- poly(p-hydroxystyrene) resin for the removal of trace cobalt from acidic solution

ABSTRACT

Trace cobalt ion in the zinc sulfate electrolyte is the most difficult to be removed among all metallic impurities and has the most detrimental effect on zinc electrowinning. In this study, poly(p-hydroxystyrene) resin was first prepared from polystyrene, and then 1-nitroso-2-naphthol was grafted onto poly(p-hydroxystyrene) resin through -O- group by a series of reactions to obtain the 1-nitroso-2-naphthol-grafted-poly(p-hydroxystyrene) resin. Finally, the grafted resin was supported on SiO₂. The supported resin could removal trace cobalt ions with good selectivity and reusability in the zinc sulfate leachate, which can meet the requirements of the industrial electrolytic zinc process.     

2-萘酚反相高效液相色谱分析

本文以反相高效液相色谱对2—萘酚及有机杂质进行分析。选择流动相，离子对，检测波长，并研究了不同牌号ODS C18色谱柱的重现性，得到了2—萘酚及杂质萘、1—萘酚、2，2’—联萘酚的相关系数分别为：０．9998；0．9990；0．9912；0．9979。标准偏差和变异系数分别为：0．2738％，0．2776％；0．00679％，1.4839％；0．00527％，1．2663％；0．007133%，1．7746%。得到了它们准确度的数据。并确定了最小检出量。     

1，1′-硫代双（2－萘酚）的合成

以2-萘酚为主要原料,与二氯化硫在甲苯、乙酸乙酯组成的混合溶剂中反应,合成了抗氧剂1,1′-硫代双（2-萘酚）。确定的最佳反应条件为：溶剂为由甲苯、乙酸乙酯组成的混合溶剂,甲苯、乙酸乙酯重量比为3：2,溶剂与2－萘酚重量比为8：1,2－萘酚与二氯化硫物质的量比为2：1．03,反应温度10-20℃,反应时间3h,产品收率84．7％,纯度大于99．0％。     

Impregnated of C6CoFeN6 nanoparticles in poly-1-naphthol for uptake of Cs(I) from aqueous waste

To carry out our research, C₆CoFeN₆@poly-1-naphthol nanoparticles were synthesized and characterized by SEM, X-ray diffraction, Fourier transform infrared, thermogravimetric analysis and Brunauer–Emmett–Teller (BET) analyses. The SEM images indicate that the average particle sizes are about 60 nm in diameter. The BET result provides a clear evidence for the high surface area of the sample 180.6 m²/g. Cs(I) ions removed from the aqueous solution in a batch mode using CoHCF@poly-1-nanphtol as an adsorbent. The adsorption effecting parameters such as the solution pH, initial Cs(I) concentration, contact time and temperature were studied. Maximum sorption capacity for the nanocomposite was found to be 200.5 mg/g at 1000 mg/g, pH = 5 and 298 K. The time-adsorption dependence studies indicated that the maximum Cs(I) uptake was within the initial 40 min contact time and the adsorption mechanism was governed by the double exponential model. The equilibrium sorption data fitted well to the Freudlich model with n ? 1 indicating a stronger interaction and high affinity of C₆CoFeN₆@poly-1-naphthol for Cs(I) ions. The thermodynamic parameters, including changes in Gibbs free energy, entropy and enthalpy, were determined. The results indicated that CoHCF–poly-1-nanphtol could be a potential adsorbent for the uptake of Cs(I) ions from an aqueous solution.     

Combination of redox capacity and double layer capacitance in composite electrodes through immobilization of an organic redox couple on carbon black

Carbon electrodes have been modified with 2-nitro-1-naphthol with the aim of producing composite supercapacitor electrodes, which make use of both the electric double layer (EDL) capacitance of high surface area carbon and the redox capacity (pseudocapacitance) of the organic compound. In situ FTIR and cyclic voltammetric data confirm literature reports of the reduction of 2-nitro-1-naphthol to 2-amino-1-naphthol and the subsequent oxidation of the o-aminonaphthol to the corresponding o-naphthaquinoneimine in aqueous acidic media. The measurements also show that the quinoneimine is not stable and hydrolized in sulphuric acid electrolyte to 1,2-naphthaquinone. The chemically highly reversible o-naphthaquinone/o-naphthahydroquinone couple remains immobilized on the carbon electrodes during redox cycling. The organic redox couple contributes a capacity of 35 mA h g⁻¹ of the bare carbon to the overall charge storage capability of the composite electrode. Surprisingly, it does not affect the capacitance of the electric double layer of the carbon. During 1000 charge/discharge cycles, the pseudocapacitance decreases by less than 20% in a normal large-volume electrochemical cell. Electrochemical impedance measurements show that the full capacity of the electrode is accessible at frequencies below 0.1 Hz.     

6-丙基-2-萘酚的合成研究

以2-萘酚为起始原料,经过O-甲基化、酰化、黄鸣龙还原、脱甲基等一系列反应,得到目标产物6-丙基-2-萘酚,总收率为52.3%。其结构经IR、1H NMR、MS分析确证。     

Porous aromatic networks with amine linkers for adsorption of hydroxylated aromatic hydrocarbons

The porous covalent organic polymers (COPs) are valuable materials in various fields such as gas storage, adsorption or separation, luminescent detection, catalysis, and sensors. Two thermally stable COPs with aromatic skeleton linked by amine groups were prepared by Buchwald–Hartwig protocol. The COPs with respective Brunauer–Emmett–Teller surface area of 204 and 178 m²/g were employed for adsorption of hydroxylated aromatic hydrocarbons (HAHs) due to expected strong π–π stacking and hydrogen-bond interactions between COPs and HAH. In adsorption of phenol from water, COP₂ showed far better capacity than COP₁, silica, basic alumina, and macroporous resin (D101). In adsorption of 2-naphthol COP₁ and COP₂ displayed similar capacity, being 2.8, 5.4, and 7.4 times high as those for macroporous resin (D101), basic alumina, and silica, respectively. COP₁ and COP₂ are useful for efficient separation of 2-naphthol or other HAHs from waste water. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 46919.     

偶氮染料的偶氮-醌腙互变异构的研究(Ⅱ)──2-苯基偶氮-1-萘酚的偶氮-醌腙异构

合成并测定11个2-苯基偶氮-l-萘酚染料的~1H、~13CNMR谱,对氢谱进行了归属,讨论了苯环上取代基的电子效应、溶剂的pH值对偶氮-醌腙互变异构以及结构对颜色的影响．     

Preparation of Silica-PAN Functionalized Nanoextractants for the Extraction of Ferbam from Various Samples

1-(2-pyridylazo)-2-naphthol modified SiO₂ nanoparticles were synthesized and evaluated as a nanoadsorbent for removing Ferbam from various environmental sources and fortified grain and vegetables samples. The 1-(2-pyridylazo)-2-naphthol modified SiO₂ nanoparticles were prepared by the sol-gel method. Nanoparticles were characterized by SEM and FT-IR. The adsorption of Ferbam was examined by the batch equilibrium technique. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions, and effects of interfering ions for the recovery of analyte were investigated. The equilibrium data analyzed by using the Langmuir isotherm, and the Freundlich and Temkin isotherm models, showed better agreement with the former model. The adsorption capacity of nanometer SiO₂-1-(2-pyridylazo)-2-naphthol was found to be 50.70 μmol/g at optimum pH and the detection limit (3σ) was 0.40 μg/L. The extractant showed rapid kinetic sorption. The adsorption equilibrium of Ferbam on nanometer SiO₂-1-(2-pyridylazo)-2-naphthol was achieved in 10 mins. Adsorbed Ferbam was easily eluted with 6 mL of 6 M hydrochloric acid. The maximum preconcentration factor was 58.33. The method was applied for the determination of trace amounts of Ferbam in various water samples and fortified samples.     

Construction of highly efficient 0D/2D Bi2MoO6/g-C3N4 heterojunctions for visible-light-driven photodegradation of 1-naphthol

Photocatalytic degradation is an ecologically benign method of reducing organic contaminants in wastewater. To remove the pollutant 1-naphthol, highly efficient 0D/2D Bi₂MoO₆/g-C₃N₄ heterojunctions were successfully assembled by a one-step hydrothermal method, where zero-dimension (0D) Bi₂MoO₆ nanoparticles were firmly bonded to two-dimension (2D) g-C₃N₄ nanosheets. 0D/2D Bi₂MoO₆/g-C₃N₄ exhibited exceptional degradation efficiency for 1-naphthol with a removal rate of 81.5% after 60 min of visible light irradiation. The enhanced photocatalytic ability was attributed to the matched band structures and tightly connected heterojunctions, which effectively prevented the recombination of photogenerated carriers. Besides, the photodegradation mechanism was revealed by investigating the catalysts' crystal phase, morphology, physicochemical and optical properties. This work introduces a novel method for one-step preparation of 0D/2D photocatalysts and advances the utilization of photodegradation for organic pollutants.     

微波辐射下1,3-二硝基-2-萘酚的合成

微波辐射下,2-萘酚与硝酸铈铵在醋酸和聚乙二醇溶液中反应生成1,3-二硝基-2-萘酚。提供了一种温和的、简便的制备1,3-二硝基-2-萘酚的一种新方法。结果表明最佳反应条件为:2-萘酚与硝酸铈铵的物质的量比为1∶1.2,辐射功率:30 W:辐射爬升时间:4.00 min;微波反应时间:4.00 min;温度:45℃(最大54℃);压力:207 kPa;1,3-二硝基-2萘酚的产率达76.4%。     

Poly (acridine orange) film modified electrode for the determination 1-naphthol in the presence of 2-naphthol

The voltammetric behavior of 1-naphthol was studied with a poly (acridine orange) (PAO) film modified glass carbon electrode (GCE). The electrooxidation of 1-naphthol was an irreversible process with its oxidation overpotential at the PAO electrode 180 mV lower than that on the GCE. PAO electrode demonstrated electrocatalytic activity to the electrooxidation of 1-naphthol giving a greatly improved detection limit down to 8 × 10⁻⁸ mol L⁻¹(S/N = 3). At the optimal experimental condition, the oxidation peak current from the PAO electrode was linearly proportional to the concentration of 1-naphthol in the range of 2 × 10⁻⁷ to 3.2 × 10⁻⁶ mol L⁻¹ and 5.2 × 10⁻⁶ to 1.2 × 10⁻⁴ mol L⁻¹. The differences of the oxidation peak potentials between 1-naphthol and the coexisted 2-naphthol was 170 mV allowing the selective detection of 1-naphthol in a mixed solution with 2-naphthol. The detection of 1-naphthol in tap water and river water was carried out with satisfactory results.     

荧光增白剂PEB的合成工艺

以β-萘酚为基本原料,在浓硫酸催化下经Reimer-Tiemann反应合成了2-羟基-1-萘甲醛,后者在醋酸酐存在下与丙二酸二乙酯反应合成了荧光增白剂PEB。在优化工艺条件下所得产品总收率达68.4％,纯度大于99％。     

高效液相色谱法测定盐酸度洛西汀中1-萘酚的含量

建立一种适用于测定盐酸度洛西汀中1-萘酚的测定方法。色谱柱为AgilentC18柱(5μm,4.6mm×250mm);磷酸盐缓冲溶液(pH=5.8)-乙腈(63∶37)为流动相;检测波长为230nm;柱温为30℃;流速1.0mL/min;进样体积为10μL。样品中盐酸度洛西汀和1-萘酚分离度良好,1-萘酚的最低检测限为0.132ng。所建立的方法简便、快速,可准确地分离盐酸度洛西汀中的1-萘酚,并能有效监控产品中的主要有关物质。     

树脂吸附法处理2-萘酚母液废水的研究

通过废水静态吸附试验,筛选出2-萘酚母液废水处理的吸附树脂,确定了2-萘酚母液废水处理的pH值,考察了废水浓度及温度对树脂平衡吸附量的影响;通过废水动态吸附试验,考察了2-萘酚母液废水流速对一级和二级吸附树脂吸附效果的影响;通过动态脱附试验,考察了脱附剂浓度、脱附剂用量和脱附温度对树脂脱附效果的影响;确定了树脂吸附法处理2-萘酚母液废水的最佳工艺参数和处理后废水的CODCr值。     

苄基-2-萘基醚的相转移催化合成研究

以四丁基溴化铵为相转移催化剂,2-萘酚和氯化苄为原料合成苄基-2-萘基醚,采用单因素实验法,得到最佳配比为2-萘酚∶氯化苄∶催化剂∶氢氧化钠=1∶1.05∶0.028∶1.10(摩尔比)。在最佳反应温度100°C下反应1.5h,苄基-2-萘基醚的收率可达到85.32%以上,产品纯度达到99.6%以上。     

2-萘酚生产废水处理技术研究进展

2-萘酚是一种重要有机中间体,其传统的浓硫酸磺化-碱熔生产工艺产生的废水量大,水质成分复杂,并会有较高价值的中间产物。从2-萘酚生产工艺过程上分析了废水来源和废水特性,综述了氧化法、浓缩法、吸附法和组合工艺对2-萘酚生产废水的处理研究进展。指出改进生产工艺,从源头减少废水排放,以及利用工厂自身的余热、余料开发低成本组合工艺实现废水处理与资源化应是以后2-萘酚生产废水处理的研究方向。     

一种新型2-羟乙基萘并噁唑化合物的合成

以2-萘酚为原料,乙腈为溶剂,反应温度为60℃,在CuCl2与3-氨基-1-丙醇形成的络合物的催化作用下合成一种新型含N芳杂环化合物,通过红外、氢谱、碳谱及质谱等检测手段,确证该化合物为2-羟乙基萘并噁唑,此合成方法具有原料易得,条件温和,操作简便等特点。     

Synthesis of novel poly[(1,3-adamantyl)bis(2-naphthol)] with low dielectric constant

A novel thermally stable and low dielectric poly(2-naphthol) containing an adamantyl unit (3) has been developed. Polymer 3 was easily prepared by oxidative coupling polymerization of (1,3-adamantyl)bis(2-naphthol) with CuCl(OH)TMEDA as a catalyst. The polymerization produced regiocontrolled polymer 3 with a number-average molecular weight of 10,500 Da and a molecular weight distribution of 4.1. The 5% weight loss temperature of polymer 3 was 480 °C and no glass transition temperature was observed. The dielectric constants (ε) of polymer 3 estimated from the refractive index and the capacitance were 2.92 and 2.96, respectively.     

MEASUREMENT OF THE DIFFUSIVITY OF 1-NAPHTHOL IN WATER WITH A ROTATING DISC

The solubility and diffusivity of 1-naphthol in water are reported at several temperatures.