氯化铜脱除硫化氢气体制硫磺研究

A novel technology of removing H2S with cupric chloride solution was developed in this paper. Cupric as the form of CuS deposition, the CuS produced was then oxidized by excessive cupric ion in another reactor meanwhile cupric ion that has been consumed can be recovered by the oxidization of with oxygen in air, and the solution can be circulated. Moreover, the leaching kinetics of CuS by cupric ion was studied. The removal efficiency of H2S is close to 100%, and the required operating condition is mild. Compared with other wet oxidiza-tion methods, no raw material is consumed except O2 in air, the process has no secondary pollution and no problem of degradation and scale, and the absorbent is much stable and reliable.     

The Effects of Oxidative Pretreatment of Zinc-containing Dust on Contents of Iron and Manganese in Ammoniacal Leaching Solution and Product ion of Zinc Oxide

The zinc-containing dust was oxidatively pretreated with calcium hypochlorite,subsequently leached with ammonia/ammonium bicarbonate solution to obtain the ammoniacal leaching solution,and zinc oxide was produced by ammonia distillation of the ammoniacal leaching solution and subsequent calcination. The elements of iron and manganese could not be detected in ammoniacal leaching solution,and the extraction rate of zinc was 98.2% in ammoniacal leaching process. The zinc oxide content in the product is 99.5%(ω),and the contents of iron and manganese in the product were 0.002 8‰ and 0.000 84‰(ω), respectively. The analyses of the valence states of iron and manganese in the zinc-containing dust with and without pretreatment were performed by chemical analysis and XPS,and the possible oxidation mechanism of the oxidative pretreatment of the dust was discussed. It is concluded that Fe 2+-oxide and Mn 2+-oxide in the dust were oxidized to Fe 3+-oxide and/or its hydrate and Mn 4+-oxide and/or its hydrate by calcium hypochlorite during the oxidative pretreatment process,respectively.     

On the database-based strategy of candidate extractant generation for de-phenol process in coking wastewater treatment

A database-based strategy of candidate generation was proposed for molecular design of new de-phenol extractants following the idea of finding new applications of existing commercial compounds. The strategy has the advantage that the environmental, safety and health risks of candidate compounds are known and controllable.In this work, the Existing Commercial Compounds (ECC) database and special combined search strategy were developed as the base for the proposed CAMD method following such idea, and molecules for phenol extraction used in coking wastewater treatment were selected from the ECC database. The candidate solvents cover the following categories: ketones, esters, ethers, alcohols, anhydrides and benzene compounds, which are consistent with the de-phenol extractants commonly used in the industry or experiment. The compounds with higher partition coefficient and selectivity than widely used methyl isobutyl ketone (MIBK) are mainly ketones. 26 obtained molecules showhigher partition coefficient and selectivity than MIBK,which are suggested to be further investigated by experiment. Furthermore, analysis of these potential moleculesmay present the effective functional groups as the initial group set to generate newmolecular structures of de-phenol extractants. The results showthat the proposedmethod enables us to efficiently generate chemicals with benefits of less time, less economical cost, and known environmental impact as well.     

Effect of Carbon Source on Crystal Morphology of SiC in-situ Formed in AI2O3-Si-C Matrix

Three kinds of Al2O3- Si- C matrix specimens were prepared using tabular corundum powder and Si powder as starting materials,ultrafine flake graphite,nano carbon black,and carbon nanotubes as carbon sources,respectively,to research the effect of micro or nano carbon materials on structure and morphology of formed Si C crystals. The specimens were fired at 1 000,1 200 and 1 400℃ for 3 h in carbon-embedded condition,respectively.The phase composition was studied by XRD and the crystal morphology of Si C was investigated by FESEM. The results show that:( 1) the amount of Si C increases with the firing temperature rising;( 2) the in-situ reaction mechanism and the formed Si C crystal morphology vary with carbon source: carbon nanotubes are generally converted into Si C whiskers by carbon nanotubes-confined reaction; Si and nano carbon black react to nucleate quickly,and the nucleated Si C crystals grow evenly in all directions forming Si C particles; Si C whiskers are produced from edge to internal of ultrafine flake graphite.     

Measurement and correlation of solubility of diosmin in four pure solvents and β-cyclodextrin solution at 298.15 K to 333.15 K

The aim of present study was to measure and correlate the solubility of poorly water-soluble flavonoid diosmin in water, ethanol, isopropyl alcohol (IPA), polyethylene glycol-400 (PEG-400) andβ-cyclodextrin (β-CD) aqueous solution (0.02 mol·L-1). The solubility of diosmin was measured using the shake flask method from (298.15 to 333.15) K at atmospheric pressure. The experimental solubilities of diosmin were regressed by the modified Apelblat model with a relative deviation in the range of 0.048%to 5.940%. The correlation coefficients were observed in the range of 0.9957 to 0.9995. The solubility of diosmin was found to be increased with temperature in all sample matrices investigated. The mole fraction solubility of diosmin was found to be higher inβ-CD aqueous solution and PEG-400 as compared to water, ethanol and IPA. Based on solubility data of present study, diosmin was considered as practical y insoluble in water, insoluble in ethanol&IPA and soluble in PEG-400 andβ-CD aqueous solution.     

Elucidating the effect of oxides on the zeolite catalyzed alkylation of benzene with 1-dodecene

In the present work, the effect of oxides on the alkylation of benzene with 1-dodecene was comprehensively investigated over MCM-49 n-heptanol, n-heptaldehyde and n-heptanoic acid were selected as the model oxides herein, and obvious decrease of lifetime could be caused by only trace amount of oxides added in the feedstocks. However, the deactivated catalysts were difficult to be regenerated by extraction with hot benzene. Additionally, coke-burning was also proved to be incapable to regenerate ...     

Biodegradation of Leather Waste by Enzymatic Treatment

The treatment of shavings, trimmings and splits of leather waste from tanneries has a potential to generate value-added products. In this study enzymatic treatment of leather waste was performed. This method utilizes alkaline protease produced by Bacillus subtilis in our laboratory by submerged fermentation. Optimum conditions of pH, time duration, temperature and concentration of enzyme were determined for maximum degradation of leather waste. The amount of degradation was measured by the release of amino acid hydroxyproline. Amino acid composition in the hydrolysate obtained by the enzyme hydrolysis was determined. This relative simple biotreatment of leather waste may provide a practical and economical solution.     

高Al_(13)含量聚合氯化铝制备γ-Al_2O_3及表征(英文)

In this paper a polyaluminum chloride solution with high Al13 content was prepared and used as raw material for preparation ofγ-Al2O3.The texture and crystalline phase of the prepared alumina samples were characterized by energy dispersive X-ray spectroscopy(EDX) ,X-ray diffraction,transmission electron microscope(TEM) and nuclear magnetic resonance(NMR) analyses.The effects of alkaline solution and calcination temperature were investigated.The results showed that alkaline solution including NH3·H2O and NaOH had little effect on the alumina sample formation.The impurities of NH4Cl and NaCl in solution can be removed through repeated washing by EDX analysis.Calcination temperature had a significant effect on alumina crystal phase.The alumina sample can transform completely toγ-Al2O3 in the subsequent heating from 600°C to 800°C.It is very interesting that Al13 can be existed inγ-Al2O3 phase even after calcinations.The results indicate that polyaluminum chloride with high Al13 content is an effective material to prepareγ-Al2O3.     

用氯甲基化脱除焦化苯中噻吩的研究

研究了用氯甲基化脱除焦化苯及轻苯中噻吩的方法,通过对噻吩基化反应的温度与原料配比的考察表明,焦化苯中的噻吩可完全转化为噻吩聚合物,在反应温度为70℃,焦化苯（含噻吩1.4g/L),甲醛：HCl=6:1:1条件下,搅拌反应3h,苯中的噻吩肿除率可达100％。     

采用反应-精馏法对焦化纯苯进行脱硫精制的研究

采用反应-精馏法对焦化纯苯中噻吩进行脱除,探讨了硫酸用量、填料层高度、填料种类及回流情况等主要影响因素对噻吩脱除率的影响。结果表明,对400mL噻吩质量浓度为0.030g/100mL的噻吩-苯溶液,采用玻璃多圈柱状填料,填料层高度为40cm,硫酸用量为80mL,人工控制回流情况,噻吩脱除率可达94%以上,苯中噻吩的质量分数小于2×10-5。     

氯气浸出硫渣制备四氯化锡

四氯化锡的生产是用精锡与氯气反应得到的。为了降低工业四氯化锡的生产成本,采用硫渣（粗锡精炼产出的一种废渣）与氯气反应,制备四氯化锡。研究了氯气浸出反应温度,反应时间,液固比,搅拌速度等因素对硫渣中锡浸出率的影响。实验结果表明,氯气能够与硫渣中的锡反应,生成四氯化锡,硫渣中锡的浸出率可以达到90%以上。最佳浸出条件：四氯化锡与硫渣的初始液固质量比为2∶1,反应温度为80～90 ℃,反应时间为6 h,搅拌速度为100 r/min。浸出液经过精馏,脱除三氯化砷、三氯化锑等杂质,实验产出的四氯化锡产品的质量达到用精锡生产的四氯化锡产品的质量标准要求。     

盐酸为氯源“一锅法”绿色高效合成α-氯噻吩

在现有氯碱工业中，以氯气为氯源的氯化反应安全性差且产生过量盐酸，氯的原子经济性较差。针对这些问题，本文以盐酸为唯一氯源，经双氧水氧化得到氯气分子，进而氯化噻吩合成α-氯噻吩（2-氯噻吩和2,5-二氯噻吩）。产物结构经气质联用分析仪（GC-MS）与核磁氢谱（¹H NMR）分析确定。通过对HCl量、H₂O₂量、反应温度和反应时间等工艺条件的考察，获得最佳实验条件为n(噻吩)∶n(HCl)∶n(H₂O₂)=1∶2.7∶2.1，反应温度35℃，反应时间3h，经气相色谱分析得到噻吩的转化率达100%，α-氯噻吩选择性达93%。另外，通过离子色谱对反应前后水相中氯离子浓度检测来确定氯离子的消耗量，并对单程反应后水相重复利用的工艺条件进行了探究。研究结果表明该工艺路线绿色安全，反应条件温和，后处理简单。水相中无其他杂质且可循环回收利用，工艺条件更适合工业化生产，同时也为氯化氢气体的回收利用提供了另外一种可能的途径。     

2,3,5-三氯吡啶醇钠的合成收率影响因素分析

本文着重研究了农药中间体2,3,5-三氯吡啶醇钠的合成影响因素。以三氯乙酰氯和丙烯晴为原料,在一定反应条件下生成长链烃后再加入催化剂氯化锌反应制得四氯吡啶,再加入氢氧化钠溶液生成2,3,5-三氯吡啶醇钠。本文研究了反应温度、时间、催化剂用量及碱液质量分数等条件对2,3,5-三氯吡啶醇钠收率的影响,并采用分步精馏分离出反应产物,不仅使后处理步骤减少,而且产品收率提高,制得三氯吡啶醇钠纯度85%以上。     

Graft copolymerization of thiophene onto polystyrene synthesized via nitroxide‐mediated polymerization and its polymer − clay nanocomposite

A new strategy for graft copolymerization of thiophene onto a polystyrene (PSt) backbone by a multi‐step process is suggested and the effects of an organoclay on the final properties of the graft copolymer sample are described. For this purpose, first poly(styrene‐co‐4‐chloromethyl styrene) [P(St‐co‐CMSt)] was synthesized via nitroxide‐mediated polymerization. Afterwards, the chlorine groups of P(St‐co‐CMSt) were converted to thiophene groups using the Kumada cross‐coupling reaction and thiophene‐functionalized PSt multicenter macromonomer (ThPStM) was synthesized. The graft copolymerization of thiophene monomers onto PSt was initiated by oxidized thiophene groups in the PSt chains after addition of ferric chloride (FeCl₃), an oxidative catalyst for polythiophene synthesis, and FeCl₃‐doped polythiophene was chemically grafted onto PSt chains via oxidation polymerization. The graft copolymer obtained was characterized by ¹H NMR and Fourier transform infrared spectroscopy, and its electroactivity behavior was verified under cyclic voltammetric conditions. Finally, PSt‐g‐PTh/montmorillonite nanocomposite was prepared by a solution intercalation method. The level of dispersion of organoclay and the microstructure of the resulting nanocomposite were probed by means of XRD and transmission electron microscopy. It was found that the addition of only a small amount of organoclay (5 wt%) was enough to improve the thermal stabilities of the nanocomposite.© 2013 Society of Chemical Industry     

液氯中重金属元素的限量检测方法

介绍一种液氯中重金属元素的限量检测方法：在弱酸性（pH值为3—4）条件下,使试样中的重金属离子与硫化钠作用,生成棕黑色悬浮物。并以采用该法检测铅标准溶液为例,进行了详细说明。     

焦化苯中噻吩在酸性沸石催化剂上的催化裂解性能

研究了焦化苯中噻吩在酸性沸石催化剂上的催化裂解性能. 结果表明：噻吩在HZSM-5沸石催化剂的作用下被分解生成硫化氢气体逸出,进而达到脱硫的目的. 通过对不同温度和压力下的催化脱硫性能进行考察,认为HZSM-5沸石催化剂对脱除苯中噻吩具有较高的活性及较好的活性稳定性,且温度、压力是影响催化剂活性和稳定性的重要因素. 以含270 mg/L噻吩的焦化苯为原料,在反应温度为320~380℃、反应压力为3.5~6.0 MPa、质量空速为4~12 h-1的条件下,能彻底脱除其中的噻吩.     

焦化轻苯回收噻吩及其衍生物的技术进展

结合作者的研究工作,概述了噻吩及其衍生物的应用前景,着重综述了实用性强、环保、经济可行的萃取精馏+吸附;萃取精馏+反应精馏;萃取精馏+离子液体络合萃取等新型组合工艺,对合理利用噻吩资源,减少焦化苯精制中的环境污染等具有十分重要的意义。     

石膏转化法生产硫酸钾的工艺研究

本文叙述以氨循环实现天然石膏或磷石膏与氯化钾一步转化制取无氯钾肥—硫酸钾的实验室试验。探讨了原料配比、氨浓度、温度等参数对氯化钾转化率的影响，得出了适宜的工艺条件。该法具有工艺简单、原料便宜易得、反应液腐蚀性小、经济效益高等优点