粉煤灰及膨润土对Ni^2＋，Zn^2＋，Cd^2＋，Pb^2＋的吸附研究

研究了粉煤灰和膨润土对溶液中有毒重金属离子Ni~(2 )、Zn~(2 )、Pb~(2 )、Cd~(2 )的吸附能力。动态吸附试验显示,吸附过程是快速的。试验结果表明:粉煤灰对Zn~(2 )的吸附能力和膨润土相当,对Ni~(2 )、Cd~(2 )的吸附能力均大于膨润土。平衡吸附模型说明在高浓度下,Ni~(2 )、Zn~(2 )、Pd~(2 )在粉煤灰中,Ni~(2 )、Pd~(2 )在膨润土中的吸附符合Langmuir模式。试验还表明:随着吸附剂中Ni~(2 )、Zn~(2 )、Pb~(2 )、Cd含量增加,粉煤灰和膨润土对Ni~(2 )、Zn~(2 )、Pb~(2 )、Cd~(2 )的吸附百分率下降。     

二叔丁基氮氧自由基对AN_MA和MMA的高效阻聚作用

用混浊法和沸腾法分别研究了二叔丁基氮氧自由基(DTBNO)对丙烯腈(AN)及丙烯酸甲酯(MA)、甲基丙烯酸甲酯(MMA)自由基聚合的阻聚作用。结果表明,DTBNO对AN有较强的阻聚作用;DTBNO与对苯二酚(HQ)、苯醌(BQ)、二乙基羟胺(DEHA)等分别组成二元混合物时,其阻聚效果非常明显。当DTBNO-DEHA和DtBNO-HQ的浓度(ppm,下同)比分别为500:1000和1000:500时,对AN的阻聚效果最好;在二元混合阻聚剂中加入适量吩噻嗪(PT),其阻聚效果更佳,如DTBNO-DEHA-PT(500:500:500)在100℃时可使MMA完全终止聚合反应。     

Activated carbon sorbent with thioetheric sites—preparation and characterization

An activated carbon sorbent containing thioetheric sites (ACTS) was prepared by modification of the activated carbon with 2,2′-thiodiethanol. The specific surface area, pore volume, concentration of oxygen-containing groups and sulfur content of the sorbent were determined. The sorption behavior towards ions of some precious metals—Au(III), Pt(IV), Pd(II) and heavy metals—Ni(II), Zn(II), Fe(III), Cu(II), Pb(II), Cd(II) and Co(II) was studied. Selectivity towards gold, palladium and platinum in the pH range 1–9 was observed. The capacity for gold was 80 mg g⁻¹. The sorption of Au(III) at pH 1 is not affected by milligram amounts of Ni(II), Zn(II), Fe(III), Cu(II), Pb(II), Cd(II) and Co(II). The sorbed gold species is Au(0).     

Synthesis of 3-oxalinolenic acid and β-oxidation-resistant 3-oxa-oxylipins

3-Oxalinolenic acid (3-oxa-9(Z), 12(Z), 15(Z)-octadecatrienoic acid or (6(Z), 9(Z), 12(Z)-pentadecatrienyloxy)acetic acid) was synthesized from 5(Z), 8(Z), 11(Z), 14(Z), 17(Z)-eicosapentaenoic acid by a sequence involving the C15 aldehyde 3(Z), 6(Z), 9(Z), 12(Z)-pentadecatetraenal as a key intermediate. Conversion of the aldehyde by isomerization and two steps of reduction afforded 6(Z), 9(Z), 12(Z)-pentadecatrienol, which was coupled to bromoacetate to afford after purification by HPLC >99%-pure 3-oxalinolenic acid in 10–15% overall yield. 3-Oxalinolenic acid was efficiently oxygenated by soybean lipoxygenase-1 into 3-oxa-13(S)-hydroperoxy-9(Z), 11(E), 15(Z)-octadecatrienoic acid, and this hydroperoxide could be further converted chemically into 3-oxa-13(S)-hydroxy-9(Z), 11(E), 15(Z)-octadecatrienoic acid and 3-oxa-13-oxo-9(Z), 11(E), 15(Z)-octadecatrienoic acid. The 3-oxa-hydroperoxide also served as the substrate for the plant enzymes allene oxide synthase, divinyl ether synthase, and hydroperoxide lyase to produce 3-oxa-12-oxo-10, 15(Z)-phytodienoic acid and other 3-oxa-oxylipins that were characterized by MS, 3-Oxalinolenic acid was not oxygenated by 9-lipoxygenase from tomato but was converted at a slow rate into 3-oxa-9(S)-hydroperoxy-10(E), 12(Z), 15(Z)-octadecatrienoic acid by recombinant maize 9-lipoxygenase. Recombinant α-dioxygenase-1 from Arabidopsis thaliana catalyzed the conversion of 3-oxalinolenic acid into a 2-hydroperoxide, which underwent spontaneous degradation into a mixture of 6,9,12-pentadecatrienol and 6,9,12-pentadecatrienyl formate. A novel α-dioxygenase from the moss Physcomitrella patens was cloned and expressed and was found to display the same activity with 3-oxalinolenic acid as Arabidopsis thaliana α-dioxygenase-1. Lipoxygenase-generated 3-oxa-oxylipins are resistant toward β-oxidation and have the potential for displaying enhanced biological activity in situations where activity is limited by metabolic degradation.     

Adsorption of water-soluble,nonionic polymers onto cellulosic fibers

The adsorption of 12 different nonionic water-soluble polymers, methylcellulose (MC), hydroxypropylcellulose (HPC), polygalactomannan (PGM), polyglycidol (PGD), polyacrylamide (PAAm), methylolated polyacrylamide (MPAAm), polymethacrylamide (PMAAm), three differently hydrolyzed poly(vinyl acetate)s (PVAs), poly(vinyl) methyl ether (PVME), and poly(vinyl pyrrolidone) (PVP) onto bleached kraft pulp (BK), unbleached kraft pulp (UK), and a groundwood pulp (MP) has been investigated under aqueous conditions with attention to the functional groups in the polymers and the chemical character of the pulps. It was found that the adsorption was often selective toward one of the pulps. In order to gain some additional information on these interactions, some adsorption experiments were also performed on acetylated pulps. Some polymers (PGD, PAAm, MPAAm, and PVA 124) having both proton donating and accepting capability were not adsorbed onto any of the pulps. This was attributed to intramolecular hydrogen bonding in these polymers. Some polymers (PVA 224, PVME, and PVP) were strongly adsorbed onto UK but not at all onto BK. It was suggested that in these cases the adsorptive interaction was between phenolic and/or catecholic groups in the lignin on the UK and proton accepting sites on the polymers. However, for three polymers (MC, PGM, and PMAAm), a more general type of hydrogen bonding interaction was considered. For some polymers (HPC, PMAAm, and PVA 420) having hydrophobic groups, it was suggested that hydrophobic interactions were important for the adsorption.     

Synthesis, characterization, and properties of an efficient and selective adsorbent to mercury (II)

The synthesis of a water-insoluble adsorbent resin was carried out by radical polymerization of [2-(methacryloyloxy)ethyl] trimethyl ammonium chloride by using ammonium peroxydisulfate as initiator and N,N′-methylene-bis-acrylamide (MBA) as crosslinking reagent. The adsorbent was characterized by elemental analyses, and FT-IR spectroscopy. The thermal stability was studied in the presence of Hg(II). The ability to bind Hg(II), Cd(II), Zn(II), Pb(II), Cu(II), Cr(III), and U(VI) as well as the maximum adsorption capacity, and elution of the Hg(II) from the loaded resin was studied. At pH 2 the adsorbent retained 95% of Hg(II) from an aqueous solution containing 1 g/L in Hg(II). The retention of other metal ions was lower than 15%. Sorption selectivity from the binary mixtures Hg(II)-Cd(II), Hg(II)-Zn(II), Hg(II)-Pb(II), and Hg(II)-Cr(III) was studied at the optimum sorption pH value. Received: 20 April 1997/Revised: 24 July 1997/Accepted: 6 August 1997     

Selective Separation of Uranium using Alizarin Red S (ARS)-Modified Anion-Exchange Resin or by Flotation of U-ARS Chelate

ABSTRACT

An alizarin red S (ARS)-modified anion-exchange resin was prepared by a simple reaction of ARS with the anion exchanger Doulite A101 and used for the efficient sorption of uranium from aqueous media. The effect of various parameters on the sorption of U(VI) (pH effect, sorption kinetics, resin capacity and breakthrough curves) was investigated. The modified resin sorbs U(VI) over a wide range of pH (2·8–5) with a maximum sorption capacity of 0·68 mmol.g^?1 at pH 3·2 to 4·0. Iron (III), Zr(IV), Ti(IV), Cu(II), and Th(IV) ions are also sorbed to different extents, but Be(II), Bi(III), Ca(II), Mg(II), Pb(II), Hg(II), Zn(II), Cd(II), AI(III), Mn(II), Co(II) and Ni(II) are not sorbed; thus, conditions for separating U(VI) from these metal ions have been identified. For eluting U(VI) from the resin, 0·2 mol.L^?1 HCl was used and the recovery recorded was as high as 99.9%. The use of ARS is extended to float uranium quantitatively and selectively from aqueous media at pH = 4 by using oleic acid as a surfactant. The different parameters affecting the flotation process have also been investigated. Uranium(VI) has been effectively separated from natural water samples and certified uranium ores using both procedures.     

包覆HNIW用WPU/SBB复合乳液的合成与表征

以异佛尔酮二异氰酸酯(IPDI)、聚氧化丙烯二醇(PPG)、苯乙烯(St)、甲基丙烯酸丁酯(BMA)和丙烯酸丁酯(BA)等为主要原料,采用种子乳液聚合法合成了WPU/SBB(水性聚氨酯/苯丙)复合乳液;然后以此为高能炸药——HNIW(六硝基六氮杂异伍兹烷)颗粒的包覆剂和胶粘剂。采用红外光谱(FT-IR)法、X-射线衍射(XRD)法及差示扫描量热分析(DSC)法等手段对WPU/SBB复合乳液的结构进行了表征,并采用扫描电镜(SEM)、特性落高值(H50)和X-射线光电子能谱(XPS)法等分析了WPU/SBB复合乳液对HNIW的包覆效果。结果表明:包覆后HNIW的H50由13.6 cm升至34.8 cm,说明该环保型WPU/SBB复合乳液对HNIW具有明显的降感作用。     

海南核果木果实脂溶性成分的GC-MS分析

采用溶剂提取法、硅胶柱层析分离,获得海南核果木果实脂溶性提取物Ⅰ和Ⅱ,结合气相色谱-质谱联用对其化学成分进行分离、鉴定及分析。结果发现,海南核果木果实脂溶性提取物Ⅰ中主要为邻苯二甲酸二(2-乙基己基)酯(64.2%)和烷烃类(23.6%);从脂溶性提取物Ⅱ中鉴定出19种成分,主要为烯烃类(1.4%)、烷烃类(22.9%)、酯类(68.0%)以及植物醇(2.8%)等,酯类为饱和脂肪酸酯(35.8%),主要为软脂酸甲酯(29.0%)和十八碳酸甲酯(6.8%),不饱和脂肪酸酯(18.6%),主要为11,14-十八碳二烯酸甲酯(10.1%)和6,11-二十碳二烯酸甲酯(8.5%),另外,还含有邻苯二甲酸二(2-乙基己基)酯(13.6%)。     

生物形态氧化铝复合高吸油树脂的合成及性能研究

本文以滤纸为模板,通过浸渍-高温煅烧法制得具有生物形态的氧化铝,利用乙烯基三乙氧基硅烷(A151)对所制备样品的表面进行疏水改性。利用悬浮聚合法制备了聚甲基丙烯酸丁酯、丙烯酸丁酯和苯乙烯的吸油树脂。根据正交实验结果,得出分散剂的用量为5 wt %、交联剂的用量为2 wt %、引发剂的用量为1.5 wt %、改性氧化铝的添加量为4 wt %,树脂的吸油倍率较原树脂有了明显的提高,而且复合树脂能够反复多次使用。对改性前后的氧化物进行红外光谱(IR)、透射电镜(TEM)、扫描电镜(SEM)以及动态疏水性分析;并对复合高吸油树脂进行扫描电镜(SEM)和热重(TG-DTA)分析。     

Removal of heavy metals and neutralisation of acid mine drainage with un-activated attapulgite

Unactivated attapulgite was characterised and utilised as an adsorbent for the removal of heavy metal and neutralisation of acid mine drainage (AMD) from a gold mine. Adsorption experiments were carried out by agitation of a fixed amount of attapulgite with a fixed volume of AMD in a thermostatic shaker for varying times. Attapulgite showed that it can neutralise acid mine drainage as the pH after 4 h was 7.11. The results showed that metal ion removal after 4 h was 100% for Cu(II) and Fe(II), 93% for Co(II), 95% for Ni(II) and 66% for Mn(II) using a 10% (w/v) attapulgite loading. The experimental data best fit the Langmuir Isotherm with maximum adsorption capacities for Cu(II), Co(II), Mn(II), Fe(II) and Ni(II) being 0.0053, 0.0044, 0.0019, 0.01, and 0.0053 mg/g, respectively. The adsorption process fitted well the pseudo first order kinetics for Co(II) and Cu(II) and pseudo second order for Ni(II), Mn(II) and Fe(II). Thermodynamic data show that Cu(II), Co(II), Fe(II) and Ni(II) adsorption was thermodynamically spontaneous whilst Mn(II) was not thermodynamically spontaneous. The process is endothermic for Cu(II), Co(II), Mn(II), and Ni(II) and exothermic for Fe(II). Spent attapulgite (attapulgite that has already been used to remove metals) could be reused twice without regeneration.     

高效液相色谱测定化妆品中的紫外线吸收剂

研究了用甲醇－四氢呋喃－水作为流动相,从Ｃ１８柱上分离和测定羟苯甲酮－５－磺酸（ＭＳ４０）、水杨酸钠、水杨酸苯酯（Ｓａｌｏｌ）、羟苯甲酮（Ｍ４０）、对－二甲酸氨基苯甲酸－２－乙基己酯（６００７）、４－叔丁基－４－甲氧基二苯甲酸甲烷（１７８９）、对－甲氧基肉桂酸－２－乙基己酯（ＭＣＸ）、水氧酸－２－乙基己酯（５８７）等８种紫外线吸收剂的色谱条件,建立了用ＨＰＬＣ测定上述物质的方法。其保留时间从２．８３ｍｉｎ（ＭＳ４０）到１５．８９ｍｉｎ（５８７）之间,回收率为９６．１％～１００．６％,相关系数ｒ≥０．９９９５。     

Rapid extraction of lead(II) from succinate media with n-octylaniline in toluene

The distribution equilibrium of lead(II) species between aqueous succinate media and n-octylaniline was studied as a function of the concentrations of extractant in organic phase, weak organic acid concentration, different diluents and effect of shaking period on extraction. The quantitative extraction of lead(II) was observed with n-octylaniline in toluene from 0.0035 to 0.0065 M sodium succinate media in the pH range 8.0–8.3. The metal ion was stripped out from organic phase with water and determined complexometrically with disodium salt of EDTA or spectrophotometrically with PAR. The extraction of lead(II) was quantitative in most aromatic solvents, such as benzene, toluene and xylene, and oxygen containing solvents, amyl alcohol and n-butanol, and also in carbon tetrachloride. The stoichiometry of the extracted species was determined on the basis of slope analysis and found to be 1:2:2 (metal: acid: extractant). As an application the system was used for selective extraction of lead(II) from its binary mixture with Zn(II), Tl(I), Tl(III), Bi(III), Al(III), Cu(II), Th(IV), U(VI), Sn(IV), Sb(III) and Ca(II). The distribution coefficient for lead(II) in succinate media was of higher magnitude than salicylate and malonate media. This developed method was successfully applied for the analysis of lead(II) in real samples such as alloys, ores and pharmaceutical materials.     

Synthesis and characterization of poly(acrylaminophosphonic-carboxyl-hydrazide) chelating fibre

The poly(acrylaminophosphonic-carboxyl-hydrazide) chelating ion exchange fibre was prepared by the amination and phosphorization reaction of the hydrazine-modified polyacrylonitrile fibre. The structure of the chelating fibre and the same fibre saturated by Cu(II) and Ag(I) ions was investigated by IR spectrometer in detail. In addition, the crystalline and surface characteristics of the chelating fibre were determined by X-ray diffraction and SEM. The higher binding capacities of the fibrous sorbent for Cu(II), Pb(II), Zn(II), Co(II), Ni(II), Hg(II), Cd(II), Mn(II), Cr(III) and Ag(I) and the effect of pH value on adsorption of the chelating fibre for Cu(II) and Hg(II) ions were examined.     

Synthesis,characterization, and properties of a selective adsorbent to mercury(II) ions

A resin containing 3‐(dimethylamine)propyl acrylate and 4‐vinylpyridine was synthesized by radical polymerization (in 1:1 mole ratio). Ammonium persulfate (0.5 mol %) and N,N′‐methylene‐bis‐acrylamide (2 mol %) were used as initiator and crosslinking reagents, respectively. The resin was characterized by Fourier transform infrared (FTIR) and ultraviolet‐visible (UV‐Vis) spectroscopy. The ability to bind Hg(II), Cd(II), Zn(II), Pb(II), Cu(II), and Cr(III) as well as the maximum adsorption capacity and elution of Hg(II) ions from the loaded resin was studied. Sorption selectivity from ternary mixture Hg(II), Cd(II), and Zn(II) was studied at the optimum sorption pH value. At pH 2 the adsorbent retained 98% of Hg(II); the retention of the other metal ions was lower than 20%. The elution assay was made in HClO₄ solutions. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 85: 2559–2563, 2002     

Selective binding of mercury ions by poly(4‐vinylpyridine) hydrochloride resin

The binding ability of poly(4‐vinylpyridine) hydrochloride resin for Cu(II), Cd(II), Zn(II), Hg(II), Pb(II), Cr(III), and U(VI) was investigated. All these ions, except Hg(II), could be not removed from aqueous solutions under the same conditions. The selective sorption of Hg(II) from mixtures of ions was observed. The elution of Hg(II) bound to the resin was also investigated using various concentrations of nitric acid and perchloric acid. Due to rapid complexation, a high mercury ion‐binding capacity, high selectivity, and ease of regenerability, the resin can be useful for the removal and recovery of mercury ions from aqueous solutions. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 1557–1562, 1999     

Synthesis,Characterization and Material Application of Novel Polyimide

Novel polyimide-II containing 8-hydroxyquinoline as pendent groups was prepared by reacting N,N′-(1,1′-biphenyl)-4,4′-diyl bismaleimide--diamine polyimide-I (BPBMDDM) with 5-chloromethyl-8-hydroxyquinoline hydrochloride (CMHQ) in the presence of base catalyst. N,N′-(1,1′-biphenyl)-4,4′-diyl bismaleimide--diamine polyimide-I (BPBMDDM) was prepared by Michael addition reaction of N,N′-(1,1′-biphenyl)-4,4′-diyl bismaleimide (BPBM) with 4,4′-diaminodiphenyl methane (DDM). The resulting polyimide-II (BPBMDDMCMHQ) was characterized by spectral techniques. Polymeric metal chelates of polyimide-II were prepared using the transition metal ions Zn(II), Cu(II), Ni(II), Co(II), and Mn(II), and were characterized. Ion-exchange properties of polyimide-II (BPBMDDMCMHQ) for Fe(III), Zn(II), Ni(II) and Cu(II) metal ions were also studied by batch-equilibration method. The polyimide-II (BPBMDDMCMHQ) has good metal uptake capacity at varying pH range and can be recycled. It has thermal stability up to 240°C.     

Heavy metal ions removal through poly(acrylamide-co-methacrylic acid) resin

The resin poly(acrylamide-co-methacrylic acid) P(AAm-co-MA) by radical polymerization was synthesized and its metal ion binding was studied using the batch and column equilibrium procedures for: Cd(II), Zn(II), Pb(II), Hg(II), Al(III), and Cr(III). Experiments were carried out at different pH, metal ion concentration, temperature, and contact time. The resin’s retention behavior was influenced by the pH. The highest retention 91% (0.248 mmol/g, 6.7 mg/g) was achieved at pH 5 for Al(III), and 87% (0.265 mmol/g, 54.9 mg/g) for Pb(II). For Hg(II), the yield was 85% (0.318 mmol/g, 63.7 mg/g) at pH 2. The metal-ion retention properties were dependent on the polymer/metal ion ratio. Under competitive conditions of Pb(II), Hg(II), and Al(III), the resin showed a higher retention of Hg(II), allowing the selective separation of this metal.     

Synthesis and adsorption properties of magnetic resin microbeads with amine and mercaptan as chelating groups

Three magnetic chelating resins containing amino and mercapto groups were prepared by the suspended condensation polymerization of 2‐chloroethoxymethyl thiirane with diamines. The magnetic resins were microbeads whose diameter was in the range of 10 to 45 μm. The structure of the resins was characterized by XPS, IR, and elemental analysis. Their adsorption properties for Hg(II), Au(III), Pd(II), Pt(IV), Ag(I), Cu(II), Zn(II), and Pb(II) were investigated. The experimental results show the magnetic resins have high affinity for Hg(II) and noble metal ions. In the competitive adsorption, the resins predominantly adsorbed Hg(II) or Pd(II) in the coexistence of Cu(II), Zn(II), and Mg(II). Desorption of Pd(II) loaded on the resins was studied by using 2M hydrochloric acid solution containing 1% thiourea as desorbent. A high desorption ratio (up to 96.5%) was observed, and repeated adsorption/desorption operations showed the probability of repeated use of the magnetic resins. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 1587–1592, 2001     

Part 8. Preparation,characterization and metal complexing of poly[(2‐hydroxyethyl)‐DL‐aspartamide] in aqueous solution

Poly[(2‐hydroxyethyl)‐DL ‐aspartamide] was synthesized by polyreaction of aspartic acid and subsequent polymer‐analogous functionalization with ethanolamine. The water‐soluble polymer was characterized by FTIR, NMR, TGA and light‐scattering measurements. The metal complexing properties of the polymer were studied for Cr(III), Fe(III), Co(II), Ni(II), Cu(II), Zn(II), Sr(II), Cd(II) and Pb(II) ions in aqueous solution using the liquid‐phase polymer‐based retention (LPR) method. According to the retention profiles of LPR, Cr(III), Fe(III), Cu(II) and Pb(II) showed a strong interaction with this polymer under these conditions, indicated by retention values of about 100 %. In contrast, Co(II), Ni(II), Zn(II), Sr(II) and Cd(II) exhibited retention values of only 50–60 % in dilute solution at pH 5. © 2000 Society of Chemical Industry