二氧化硫脲合成工艺条件研究

采用双氧水(过氧化氢)与硫脲反应制备二氧化硫脲。实验以二氧化硫脲收率为指标,通过对影响二氧化硫脲收率的主要影响条件:物料配比、预置蒸馏水用量、反应温度、醇的含量等因素进行了考察,同时,利用红外色谱仪和紫外分光光度计分别对产品二氧化硫脲进行了定性分析和定量分析,通过用Origin作图,得出较好的合成条件及参数。对二氧化硫脲的工艺条件及参数进行优化,得出较好的合成条件及参数。结果表明,合成二氧化硫脲的较优工艺条件及参数为:过氧化氢与硫脲的摩尔比为2.1,溶剂蒸馏水与硫脲质量比为1,反应温度5～7℃,溶剂醇与醇水质量比为0.5。     

Fe~(2+)-H_2O_2-二氧化硫脲引发绒毛浆与MMA接枝共聚的研究

研究了Fe2+-H2O2-二氧化硫脲体系引发绒毛浆与甲基丙烯酸甲酯的接枝共聚。考察了该引发体系下反应温度、反应时间、过氧化氢用量、二氧化硫脲用量、单体浓度和液比对接枝率和接枝效率的影响。并用红外光谱对接枝纤维产物进行了鉴定。结果表明,二氧化硫脲的加入能有效地使接枝共聚得以顺利进行;适当地提高温度,增加单体浓度,控制合适的二氧化硫脲用量都能提高接枝率和接枝效率,并在较短的时间就能成功接枝;接枝效率几乎不受液比的影响,一般维持在90%以上,接枝过程产生的均聚物极少。     

二氧化硫脲还原法制备纳米铜颗粒

以CuSO4×5H2O为原料、聚乙烯吡咯烷酮为分散剂、葡萄糖和二氧化硫脲为还原剂,采用液相两步还原法制备分散性较好的球形纳米铜粉,考察了预还原步骤、二氧化硫脲与铜离子浓度配比、反应温度和反应时间对铜粉粒度、分散性和形貌的影响,表征了铜粉的特性. 结果表明,较优的制备条件为：二氧化硫脲与硫酸铜溶液浓度比2:1、反应温度75℃、反应时间15 min,该条件下所制产品为粒径20~100 nm的类球形铜粉.     

过氧化氢合成二氧化硫脲研究进展

评述以水为溶剂间歇法合成二氧化硫脲的工艺,介绍了在提高收率、延长产品保质期等方面的技术状况和最新进展,讨论了影响产品收率的因素,如物料百分比,溶剂,反应温度,反应时间,添加剂种类,投料方式,pH值等。并对我国二氧化硫脲产业发展进行了展望。     

酸浸-液相还原法从废细电线中制备微细铜粉的研究

采用酸浸法从破碎的废细电线中浸出铜,考察了初始酸浓度、反应温度、反应时间、固液比和浸出助剂对浸出率的影响。结果表明,在硝酸浓度为3.5 mol/L、过氧化氢质量分数为30%、固液比为1∶6、温度为35℃、时间为2 h条件下,铜浸出率为73.1%。再以浸出溶液为原料,聚乙烯吡咯烷酮为分散剂,葡萄糖和二氧化硫脲为还原剂,采用液相还原法制备微细铜粉,考察了二氧化硫脲和铜离子浓度比、反应温度和反应时间对铜粉粒度的影响,利用激光纳米粒度仪、X射线衍射仪、扫描电子显微镜和红外可见分光光度计对铜粉进行表征。结果表明,二氧化硫脲与铜离子浓度比为2∶1、反应时间为15 min、反应温度为75℃的条件下,可以制得分散性较好、粒径约为200~500 nm的微细铜粉。     

K301型高锰酸盐指数在线自动监测仪测定方法的探讨

从反应体系的酸度、反应时间和反应温度3个方面对K301型在线高锰酸盐指数测定方法进行了研究。结果表明：在同一酸度和反应温度下,高锰酸盐指数测定值随反应时间的廷长而逐渐增大和随反应温度的增大而逐渐增大;在相同反应温度和反应时间内,高锰酸盐指数测定值随反应酸度的增大而逐渐增大。综合以上2条件试验得出,加入8mL硫酸,反应时间为10min,反应温度为95℃,测得的高锰酸盐指数与国标方法（GB11892—89）测定结果无显著差异。     

硫脲法制备二氧化硫脲

一、概述硫脲制二氧化硫脲,此法系采用硫脲与双氧水作用,在控制一定的pH值下,析出二氧化硫脲沉淀,然后经快速脱水、洗涤、干燥。上述氧化反应过程似乎并不复杂,但从工业生产角度来看,保证和提高二氧化硫脲的收率是降低生产成本的关键。二氧化硫脲的收率与固液比、反应温度、作用时间、pH等工艺因素密切相关。     

助熔剂硅石及钾页岩对磷矿碳热还原反应的影响

考察了硅石及钾页岩分别作为助熔剂时对磷矿碳热还原反应的影响.通过考察反应温度、反应时间、烟煤过剩系数和酸度值,研究两种助熔剂对磷转化率的影响.结果表明,随着反应温度的升高、反应时间的延长、烟煤过剩系数的增大,磷的转化率逐渐提高,最后趋于稳定.随着酸度值的增大,磷的转化率呈现先增大后减小的趋势.当反应温度为1400℃,反应时间为40 min,酸度值为1.02,无烟煤过剩系数为1.5时,硅石、钾页岩作为助熔剂时磷的转化率分别达到94.50％,95.31％.通过考察残渣特性,得出钾页岩作为助熔剂时,其残渣的流动温度较硅石降低了52℃,粘度摊开面积是硅石体系的2.25倍.     

糠醛液相氧化合成富马酸的研究

究了ＫＣＩＯ３／糠醛及Ｖ２Ｏ５／ＭｏＯ３摩尔比，反应温度，反应体系酸度，相转移催化剂，反应时间等因素对糠醛液相氧化合成富马酸的影响。实验证明反应温度，反应体系的酸度，ＴＥＢＡＣ相转移催化剂用量是影响富马酸收率的主要因素。找出了最佳反应条件。富马酸收率８２．９％，高于文献报道的最高收率（８２．１８％），反应时间从文献报道的１０ｈ缩短到２ｈ。     

纤维素接枝甲基丙烯酸乙酯的合成及表征

在过氧化氢和亚铁离子组成的氧化还原体系中加入第三组分二氧化硫脲(TD),将单体甲基丙烯酸乙酯(EMA)接枝于纤维素纤维上。探讨了单体EMA用量、过氧化氢用量、TD用量、反应温度、反应时间、去离子水用量等因素对接枝率、接枝效率的影响。结果显示纤维素接枝EMA的最佳工艺条件为:纤维8 g,EMA 6 g,过氧化氢0.02 g,TD 0.5 g,去离子水150 mL,反应温度50℃,反应时间1 h。红外光谱、扫描电镜分析均表明EMA接枝到了纤维素结构上。     

Bitumen chemical modification by thiourea dioxide

This work evaluates a novel bitumen modification through the use of a chemical agent, thiourea dioxide, substance which has been traditionally used as a reducing agent. Thermo-gravimetric analysis demonstrated the formation of new chemical compounds, most probably originated through reactions between products from thiourea dioxide thermal decomposition and some highly polar bitumen molecules. As a result of these reactions, which continues even after 60 days, bitumen permanent deformation resistance at high temperature is enhanced, as indicated by a significant increase in its viscosity and elastic features. On the other hand, thiourea dioxide addition produces changes in the bitumen colloidal nature, which improve its flexibility at low in-service temperatures, and consequently its resistance to thermal cracking under loading. In fact, dynamic bending tests indicated a remarkable decrease in the value of binder glass transition temperature, which was further corroborated by differential scanning calorimetry. As a conclusion, thiourea dioxide can be seen as a promising modifying agent, which can extend the in-service temperature range at which bitumen would present a satisfactory performance.     

Performance,optimization, and mechanism of nitric oxide removal by thiourea dioxide/FeIIEDTA reaction systems

In this work, a new innovative absorption system containing both thiourea dioxide (TD) and Fe^ⅡEDTA was used to NO removal. The independently influences of O₂ volume concentration, TD concentration, original pH value and absorbent temperature on NO removal in bubbling device were examined preliminarily. The results revealed that the NO removal efficiency firstly increased and then decreased with the increasing of the three independent variables (O₂ volume concentration, TD concentration and temperature). However, the NO removal efficiency monotonously increased to some extent with pH value increasing from 6.5 to 10.5. In addition, the respective effects of the four variables and the interactive function of them on NO removal were checked with the response surface methodology (RSM) by central composite design (CCD). The calculative model showed that pH value possessed a main positive independent impact on NO removal. Furthermore, the interactive effects between any two factors were expounded by the 3D surface and counter plots. Finally, the optimum absorption conditions for the maximum NO removal at 94.3% experimentally and 95.8% statistically were obtained in O₂ volume content of 6.0%, TD concentration of 0.02 mol·L^-1, original pH value of 10.5 and absorption temperature of 42 ℃.     

硫脲法浸出废弃电脑线路板中金的研究

废弃电脑线路板是一种典型的电子废弃物,其中含有丰富的贵金属资源,而金的回收是废弃电脑线路板资源化研究的热点。研究了用硫脲浸出废弃电脑线路板中的金,考察了硫脲质量浓度、反应时间、反应温度、三价铁离子质量分数、溶液pH对金浸出率的影响。结果表明,在硫脲质量浓度为12 g/L、反应时间为60 min、反应温度为30 ℃、三价铁离子质量分数为0.45%、溶液pH为1.5条件下,金的浸出率达到90.93%。硫脲法浸金因具有浸出速率快、浸出时无毒、对环境污染小、试剂易再生、干扰离子少等优点而具有广泛的应用前景。     

Performance,optimization, and mechanism of nitric oxide removal by thiourea dioxide/FeIIEDTA reaction systems

In this work, a new innovative absorption system containing both thiourea dioxide (TD) and Fe^IIEDTA was used to NO removal. The independently influences of O₂ volume concentration, TD concentration, original pH value and absorbent temperature on NO removal in bubbling device were examined preliminarily. The results revealed that the NO removal efficiency firstly increased and then decreased with the increasing of the three independent variables (O₂ volume concentration, TD concentration and temperature). However, the NO removal efficiency monotonously increased to some extent with pH value increasing from 6.5 to 10.5. In addition, the respective effects of the four variables and the interactive function of them on NO removal were checked with the response surface methodology (RSM) by central composite design (CCD). The calculative model showed that pH value possessed a main positive independent impact on NO removal. Furthermore, the interactive effects between any two factors were expounded by the 3D surface and counter plots. Finally, the optimum absorption conditions for the maximum NO removal at 94.3% experimentally and 95.8% statistically were obtained in O₂ volume content of 6.0%, TD concentration of 0.02 mol·L⁻¹, original pH value of 10.5 and absorption temperature of 42 °C.     

载硫脲树脂对Pd~(2+)的吸附与脱附性能

研究了717载硫脲树脂对Pd2+的吸附热力学、动力学及脱附特性,考察了吸附时间、pH值、温度等因素对树脂吸附Pd2+的影响。结果表明:在pH=1—5时,吸附能力最好;等温吸附服从Freundlich经验式,在303—313 K条件下,Pd2+吸附量(质量比)为60—80 mg/g的吸附焓变为-29.24—-23.98 kJ/mol,自由能变为-8.00—-7.65 kJ/mol,吸附熵变为-70.10—-52.17 J/(K.mol)。吸附动力学符合Lagergren一级速率方程,303 K时吸附速率常数为0.022 min-1,颗粒内扩散是速率控制步骤之一,膜扩散也共同影响着吸附过程。303 K下树脂静态累积饱和吸附量为144.2 mg/g。用质量分数8%硫脲-1 mol/L HCl混合液可以将树脂上的Pd2+完全解吸。     

Study of the application of modified thiourea dioxide discharge agent in D5 non‐aqueous medium

In view of the low solubility of thiourea dioxide in water and its inertia to most chemical reagents, a novel non‐aqueous medium, decamethylcyclopentasiloxane, was introduced to replace water in the grinding process for better dispersibility and discharge stability. In this study, the effects of different grinding methods on the particle size distribution and surface appearance of thiourea dioxide were studied. The influences of aqueous and decamethylcyclopentasiloxane media on the discharge stability of thiourea dioxide in discharge paste were compared. The whiteness, handle, and the tensile strength of the discharge‐printed fabric were evaluated. The results showed that the wet grinding process endowed thiourea dioxide with smaller particle sizes and narrower size distributions in the presence of dispersants. Decamethylcyclopentasiloxane as a non‐aqueous medium was beneficial in maintaining good discharge stability of thiourea dioxide for a longer time. The fabrics discharged by the prepared thiourea dioxide printing paste had favourable whiteness, good handle, and acceptable tensile strength.     

Fe2+液相催化氧化脱除烟气中SO2

提出了一种烟气脱硫新工艺。实验选用水作脱硫剂 ,在只以Fe为催化剂的条件下进行。加入吸收液槽中的铁屑可与脱硫产生的稀硫酸进行反应 ,不仅可维持较高的吸收液pH值 ,而且产生的Fe2 + 引发了液相催化氧化SO2 反应。连续运行实验结果表明脱硫过程在不同阶段分别受SO2 溶解、Fe2 + 液相催化氧化SO2 反应、气相中SO2 扩散和铁屑与酸反应控制。吸收液中Fe2 + 质量浓度的变化和初始Fe2 + 质量浓度对脱硫率及吸收液pH值影响显示 ,可直接由清水制取高浓度硫酸亚铁溶液。实验还调查了SO2 入口质量浓度、液气比、空塔气速和吸收温度对脱硫率和吸收液pH值的影响     

响应面优化改进硫脲法浸出炼锌渣中银的工艺

采用改进硫脲法浸出含硫铁矿炼锌渣中银,用响应面方法研究了双氧水浓度［X1/（mol·L-1）］、硝酸浓度［X2/（mol·L-1）］、硫脲浓度［X3/（mol·L-1）］和浸出温度（X4/℃）对银浸出率（Y/%）的影响,并优化了浸出工艺。银浸出率与工艺因素之间的关系符合二次模型：Y=-476.0-40.17X1+58.20X2+82.15X3+12.30X4-22.65X1X3+5.03X1X4-0.51X2X4-1.08X3X4-81.47X12-3.65X22-1.30X32- 0.11X42。双氧水浓度和硫脲浓度的一次项对浸出率的影响不显著,浸出温度的一次项、双氧水浓度和硫脲浓度的二次项对浸出率有着显著影响,硝酸初始浓度的一次项和二次项对浸出率有着高度显著影响。双氧水浓度与硫脲浓度,温度与双氧水浓度、硝酸浓度、硫脲浓度之间均存在高度显著的交互作用。模型拟合所得最优的浸出条件为：双氧水浓度为0.96 mol/L、硝酸浓度为4.12 mol/L、硫脲浓度为2.17 mol/L、浸出温度为55 ℃。此条件下,银浸出率为91.3%,接近模型预测值（92.7%）。与单因素实验相比,银浸出率提高近10%。     

改进硫脲法浸出含硫铁矿炼锌渣中银的工艺

采用硫脲为络合剂、双氧水为氧化剂,研究了在硝酸介质中浸出含硫铁矿炼锌渣中银的工艺。考察了搅拌速率、反应时间、反应温度、硝酸初始浓度、双氧水浓度、硫脲浓度等因素对银浸出率的影响。结果表明,银的浸出率随着搅拌速率的增大和反应时间的延长先增大然后保持不变,随反应温度、硫脲浓度、双氧水浓度和硝酸初始浓度的增加先增大后减小。当搅拌速率为200 r/min、硝酸浓度为4.11 mol/L、双氧水浓度为0.82 mol/L、硫脲浓度为3.25 mol/L、反应温度为50 ℃、反应时间为1 h时,银浸出率可达82.0%。