Amine-functionalized mesoporous UiO-66 aerogel for CO_(2) adsorption

A mesoporous UiO-66-NH_(2) aerogel is prepared via a straightforward sol-gel method without using any binders or mechanical pressures, in which the amine groups are directly introduced into the matrix by using 2-aminoterephthalic acid. The novel UiO-66-NH_(2) aerogel also exhibits high specific surface area and mesopore-dominated structure, implying its highly potential use in CO_(2) adsorption. For ulteriorly investigating the effect of amine loading on the CO_(2) adsorption ability, a series of UiO-66-NH_(2) aerogel with different amino content is fabricated by changing the ligand/metal molar ratio. When the molar ratio is 1.45, the CO_(2) adsorption capacity reaches the optimum value of 2.13 mmol·g^(-1) at 25 ℃ and 0.1 MPa, which is 12.2% higher than that of pure UiO-66 aerogel. Additionally, UiO-66-NH_(2)-1.45 aerogel also has noticeable CO_(2) selectivity against N_(2) and CH_(4) as well as good regeneration stability. Such results imply that it has good application prospect in the field of CO_(2) adsorption, and also contains the potential to be applied in catalysis, separation and other fields.

Development of a rapid GC-FID method to simultaneously determine triethylamine, diisopropylamine, and 1,1,3,3-tetramethylguanidine residues in an active pharmaceutical ingredient

A rapid GC-FID method was developed to simultaneously determine residual levels of triethylamine(TEA), 1,1,3,3-tetramethylguanidine(TMG), and diisopropylamine(DIPA) in the synthetic route of an active pharmaceutical ingredient(API). Due to the severe absorption of amines on GC stationary phases,GC columns with various stationary phases were evaluated for optimal peak shape and reproducibility.The final conditions used the Agilent CP-Volamine column to resolve the three amines in 12 min. Various inlet liners were also screened to further improve the sensitivity of the analysis. The Restek Siltek~? liner was selected to achieve the desired detectability for the method. The quantitation limits were 4, 3, and 4 mg/mL for TEA, DIPA, and TMG in the presence of API, respectively. All three amines showed good linearity(r > 0.999) and recoveries(> 90%) over the concentration range of 3 to 16 mg/mL. The testing of residual amines was initially performed at the penultimate stage of the synthesis. However, this work demonstrates that TMG can act as a proton sponge to react with salicylic acid, the counter ion of the penultimate, to form a volatile component that elutes at a different retention time. Consequently, in the final method, these three amines were monitored in the final API to circumvent the matrix interference.Key parameters of the method were qualified per method validation requirements in ICH guidelines. The method was successfully applied for batch testing during development and implemented as an inprocess control procedure at manufacturing sites.

Facile synthesis of hydrochar-supported catalysts from glucose and its catalytic activity towards the production of functional amines

Since the utilization of abundant biomass to develop advanced materials has become an utmost priority in recent years,we developed two sustainable routes(i.e.,the impregnation method and the one-pot synthesis)to prepare the hydrochar-supported catalysts and tested its catalytic performance on the reductive amination.Several techniques,such as TEM,XRD and XPS,were adopted to characterize the structural and catalytic features of samples.Results indicated that the impregnation method favors the formation of outer-sphere surface complexes with porous structure as well as well-distributed metallic nanoparticles,while the one-pot synthesis tends to form the inner-sphere surface complexes with relatively smooth appearance and amorphous metals.This difference explains the better activity of catalysts prepared by the impregnation method which can selectively convert benzaldehyde to benzylamine with an excellent yield of 93.7%under the optimal reaction conditions;in contrast,the catalyst prepared by the one-pot synthesis only exhibits a low selectivity near to zero.Furthermore,the gram-scale test catalyzed by the same catalysts exhibits a similar yield of benzylamine in comparison to its smaller scale,which is comparable to the previously reported heterogeneous noble-based catalysts.More surprisingly,the prepared catalysts can be expediently recycled by a magnetic bar and remain the satisfying catalytic activity after reusing up to five times.In conclusion,these developed catalysts enable the synthesis of functional amines with excellent selectivity and carbon balance,proving cost-effective and sustainable access to the wide application of reductive amination.

HPLC Determination of the Major Non-protein Amino Acids and Common Biogenic Amines in Lathyrus sativus Using a Novel Extraction Method

An assay is presented for simultaneously determining 5 biogenic amines and the major non-protein amino acids: the toxin β-N-oxalyl-L-α,β-diaminopropanoic acid (β-ODAP), its isomer α-ODAP and homoarginine in Lathyrus sativus extracts using the HPLC system after derivatization with para-nitrobenzyloxycarbonyl chloride (PNZ-Cl). However, it is more worthy of noting that this paper also describes a new extraction method using 0.2 mol/L HClO4. The new method has some advantages: shorter extraction-time, simultaneous extraction of free amino acids and polyamines, better inhibiting the isomerization of β-ODAP to α-ODAP, and so on.

Bioactive Amines: Aspects of Quality and Safety in Food

Presented in several types of food, bioactive amines are described as organic bases of low molecular weight. They have vasoactive, psychoactive and toxicological characteristics and constitute a potential health risk. The concentration of amines formed in foods depends on the type of microorganisms present, the action of decarboxylase enzymes produced by microorganisms on specific amino acids and favorable conditions for enzymatic activity. The presence of these chemical metabolites has been suggested as a quality indicator in routine analyzes for food production and marketing monitoring. The detection of bioactive amines can be performed by chromatographic methods, fluorometric and enzymatic kits. Bioactive amine formation can be prevented mainly through the adoption of good manufacturing practices, but the industry can also use other methods such as temperature control in the production chain, modified atmosphere packaging and food irradiation. This review aims to address the formation of bioactive amines in foods, emphasizing the formation and classification of these metabolites, aspects related to health, acceptable limits, detection methods and control methods used in the industry to ensure food safety and quality. The success of this approach is linked to the importance of bioactive amines as quality indicators, as well as the discussion on the development of methodologies for determining these substances and discussion of acceptable parameters in food.

Study on Industrial Application of Hydrogen Sulfide Removal by Wet Oxidation Method with High Gravity Technology

The removal of hydrogen sulfide from gas plays an important role in rational utilization of resources and environ- mental protection. In this paper, the process of hydrogen sulfide removal by wet oxidation method in a rotating packed bed was investigated in a scale for treating 10 000 Nm3/h of gas. On the basis of studying the influence of the species and con- centration of alkali source, the liquid/gas volume ratio, the high gravity factor, and the hydrogen sulfide content in feed gas on the desulfurization effect, the suitable technological conditions were obtained. The hydrogen sulfide removal efficiency could reach 98.0% under these conditions. The results of continuous operation of process facilities showed that the high gravity method has many merits including higher desulfurization rate, good stability in operation, lower liquid/gas volume ratio, greater operation elasticity, and apparent energy saving effects.

Flow-Based Iodometric Extraction Method by the Hollow Fiber Membrane for the Determination of Selenium Sulfide Levels in Cosmeceutical Products

A flow-based iodometric extraction method for the determination of selenium sulfide was developed and applied to cosmeceutical products. Iodine which was generated from the reduction of selenium（IV） ions by iodide ion was on-line extracted using a polypropylene HFM （hollow fiber membrane） liquid extraction technique. The HFM extraction unit was constructed and used to support an organic solvent （hexane） and separate between the organic phase and aqueous phase. The resulting purple extract was carried to a fiber optic spectrophotometric detector for the measurement at 521 nm. Parameters which affected the extraction efficiency, sensitivity and sample throughput such as iodide （selenium molar ratio, extraction time and washing time between the cycles） were investigated and optimized. A linear dynamic range of 80-373 mg.Lt selenium solution was obtained with an extraction time of 60 sec. The total analysis time including washing was about 180 sec which provided a sample throughput of approximately 20 samples＇hr1 and excluded the sample pre-treatment. The recoveries for the determination of selenium in the forms of selenium dioxide and selenium sulfide were in the range of 103%-104% with 1%-3% RSD （relative standard deviation）. The relative errors of this method which was applied for determination of selenium sulfide levels in an anti-dandruff shampoo and a cosmeceutical bead sample were both less than 2.5%.

Synthesis of ITO Nanoparticles Prepared by the Degradation of Sulfide Method

Indium tin oxide (ITO) nanoparticles are synthesized by the two-degradation sulfide and liquid-phase co-precipitation method under the given conditions with solutions of InCl3·4H2O and SnCl4·5H2O in the presence of ethylendyamine.The sample powders were characterized by x-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses after heat treatments.The SEM results show that the size of the ITO particles prepared by the coprecipitation method is decreased to 100nm,whereas the size of the ITO prepared by degradation of sulfide increases to 1μm after heat treatment.The XRD results reveal that the size of crystallite ITO particles is increased with increasing annealing temperature.Finally the intensity ratio of I400/I222 has an increase of 29.07%for ITO prepared by the co-precipitation method.

Glycerol-Based Carbon-SO₃H Catalyzed Benign Synthetic Protocol for the Acetylation of Alcohols, Phenols and Amines under Solvent-Free Conditions

A simple and efficient solvent-free method was developed for the acetylation of alcohols, phenols and amines in excellent yields employing glycerol-based sulfonic acid (-SO3H) functionalized carbon catalyst under environmentally benign reaction conditions. The salient features of this protocol are the short reaction time, ease of product isolation and reusability of the carbon catalyst.

One-step Eco-friendly Fabrication of Antibacterial Polyester Via On-line Amination Reaction by Melt Coextrusion

The work is dedicated to develop a one-step eco-friendly method to prepare antibacterial polyethylene terephthalate(PET).We report a one-step eco-friendly method to manufacture antibacterial PET via on-line amination reaction by melt coextrusion.Beside evenly mixing of poly(hexamethylene guanidine)(PHMG)and PET in the melt coextrusion procedure,the amination reaction also occurred between PHMG and PET under high temperature(230-270℃).The antibacterial ability of composite PET showed obvious PHMG concentration dependence,and antibacterial activity reached more than 99%when PHMG content was 2.5 wt%.Moreover,LIVE/DEAD fluorescence test further confirmed that the composite PET could kill bacteria quickly and efiectively(within 30 min);while negligible cytotoxicity was observed to HSF and HUVEC cells.Onestep eco-friendly fabrication of composite antibacterial PET was accomplished by on-line melt coextrusion.The composite antibacterial PET has potential use in multiple fields to combat with pathogenic including textiles,packaging materials,decoration materials and biomedical devices,etc.

基于改进络合铁法的含硫化氢尾气处理工艺模拟与优化

目的有效处理含硫尾气,确保装置“安、稳、长、满、优”运行。方法采用Aspen Plus V11软件基于Peng-Robinson热力学模型对改进络合铁装置的H_(2)S处理过程进行了全流程模拟,并根据Box-Behnken Design对其进行了响应面设计,得到了最佳H_(2)S脱除率及其对应的优化操作参数。结果此模拟流程能够较好地反映改进络合铁装置的实际运行情况,可以作为后续优化研究的基础模型。当循环溶液温度为47.2℃、循环溶液中Fe^(3+)质量分数为8.4100%、循环溶液体积流量为3.12 m^(3)/h、电解槽电压为0.64 V时,改进络合铁装置的H_(2)S脱除率高达99.999988%。此时,外排气中H_(2)S质量浓度为9.5 mg/m^(3),完全可以满足外排气中H_(2)S质量浓度不大于10 mg/m^(3)的约束条件;t检验结果表明,采用响应面法优化得到的预测值和验证值之间不存在显著差异,其准确度一致。结论该研究结果可为进一步提升含H_(2)S尾气处理水平提供准确、可靠的理论支撑和数据来源。

硫化—胺法浮选菱锌矿体系中两相和三相泡沫的性能研究

硫化—胺法是氧化锌的主要选别方法之一,在工业生产中的指标较好,但存在浮选泡沫发黏、难消泡的问题。研究了硫化-胺法浮选菱锌矿体系中两相泡沫和三相泡沫的性能,考察了硫化钠用量、十二胺用量、矿物含量、矿物粒度、矿物种类等对泡沫稳定性的影响,并测试了不同矿物含量的矿浆黏度。结果表明,在采用硫化—胺法浮选菱锌矿时,加入硫化钠能够提高两相和三相泡沫的稳定性。不同粒度的矿物颗粒对泡沫稳定性影响不同,加入-74+37μm粒级的菱锌矿和石英颗粒均能够降低泡沫稳定性,而加入-37μm粒级的菱锌矿和石英颗粒均能够提高泡沫稳定性,-18μm的石英颗粒影响尤为明显。当十二胺与微细粒级石英共同存在时,浮选泡沫尤为稳定。加入石英颗粒后的三相泡沫半衰期均高于菱锌矿,这是由于石英矿浆的黏度高于菱锌矿,因而泡沫液膜的Marangoni效应增强,导致排液速率变慢,泡沫液膜变薄速率下降,泡沫稳定性更强。

PEI功能化乙酸锌辅助机械化学法合成的ZIF-8吸附CO_(2)性能研究

为开发高效且适合大规模生产的CO_(2)吸附剂,采用乙酸锌为辅助研磨物,ZnO为金属前驱体,利用机械化学法高效合成高比表面积的ZIF-8材料,考察了机械化学法的合成条件及优势,采用湿浸渍法将聚乙烯亚胺(PEI)负载到ZIF-8材料中,通过X射线衍射(XRD)、扫描电镜(SEM)、红外光谱(FT-IR)和N2吸附-脱附等进行表征,评价其CO_(2)吸附性能。结果表明:机械化学法可在短时间内高效合成ZIF-8材料,其收率高达80.7%。机械化学法显著减少了有机溶剂和有机配体的用量,所合成的ZIF-8具有更小的粒径。PEI的加入显著提高了ZIF-8的CO_(2)吸附性能,其中PEI负载量为60%(质量分数)的吸附剂在50℃的吸附量最高,达到90.21 mg/g,较ZIF-8提高约14倍。此外,该复合材料还表现出良好的稳定性和再生性,在CO_(2)吸附领域具有广阔的应用前景。

煤层H_(2)S与煤脱硫协同治理研究

为研究煤层H_(2)S与煤脱硫的协同治理,自制装置对复配碱液进行H_(2)S吸收和煤脱硫试验。采用离子色谱法、X射线光电子能谱、形态硫测试对吸收液和煤样进行表征,分析协同治理机理,利用响应面法分析各因素对H_(2)S吸收和煤脱硫的影响程度。结果显示:单一碱液均可吸收H_(2)S,但脱硫效果微弱;添加NaClO后,协同治理效果显著且能避免H_(2)S二次逸散,其中NaOH+NaClO协同治理效果最优。在反应后,H_(2)S及煤中低价态硫噻吩、硫醇和硫醚减少,吸收液中SO_(4)^(2-)及煤中高价态硫(亚)砜增加,表明NaOH为元素硫歧化提供碱性条件,元素硫继而被NaClO氧化。NaOH质量浓度对H_(2)S吸收影响最大,NaClO质量浓度对煤脱硫影响最大,NaOH和NaClO交互对煤脱硫与H_(2)S吸收影响显著。利用Design-Expert软件确定最佳参数:NaOH质量浓度为54 g/L、NaClO质量浓度为54 g/L、温度为21.4℃。

石灰回转窑真实烟气条件下有机胺法CO_(2)捕集试验

为推动有机胺法CO_(2)捕集工艺在钢铁行业的应用,在石灰石回转窑炉真实烟气条件下开展了有机胺法CO_(2)捕集侧线试验,考察了有机胺溶液质量分数、烟气流量、溶液喷淋量、吸收温度、油浴温度和再生压力等关键参数对捕集系统CO_(2)捕集性能的影响。结果表明,在最优试验条件(有机胺溶液质量分数为25.0%、烟气流量为20m^(3)/h、溶液喷淋量为70L/h、吸收温度为30℃、油浴温度为115℃以及再生压力为10kPa)下,捕集系统CO_(2)捕集率和解吸酸气量分别为94%和1.22m^(3)/h。在最优试验条件下进行的480h连续试验结果显示,捕集系统CO_(2)捕集率平均值为94%,解吸酸气量平均值为1.22m^(3)/h,CO_(2)捕集系统表现出良好的稳定性,证明有机胺法应用于石灰回转窑烟气CO_(2)捕集技术可行。

低碳脂肪胺的治理技术研究进展

低碳脂肪胺(LCFAs)的末端处理技术主要分为物理法、化学法和生物法等3类,物理方法主要包括液相吸收法、吸附法、空气吹脱法、膜分离法;化学法主要包括低温等离子体法、高温催化氧化、光催化氧化、微波辐射法和液相高级氧化法。重点介绍各种方法的原理、处理效率和优缺点等。研究表明,LCFAs的去除方法虽然多样,但每种方法在不同程度上都存在一定局限性。鉴于LCFAs出色的水溶性,提出将液相吸收法与高级氧化法/生物法联合使用将是一种十分具有前景的LCFAs治理技术。最后对LCFAs未来的治理方向提出了展望。

Al掺杂硫铟锌光催化剂的制备综合实验教学设计与实践

结合化学工程与工艺专业人才培养方案和实践教学体系的要求,设计了硫铟锌(ZnIn2S4)基光催化剂的制备综合性实验。实验采用溶剂热法制备了Al掺杂硫铟锌光催化剂,系统地表征分析了光催化剂的晶体结构、形貌以及光电化学特性。该实验是将典型的科研成果转化为实验教学内容,有助于学生了解该领域的前沿科学成果和研究方法,掌握光催化剂的制备技术,进而深入理解光电化学性能相关专业理论知识。科研反哺教学有利于创新实验教学内容,激发和培养学生的创新意识和专业综合实践能力。

酿造调味品中生物胺分析与控制研究进展

酿造调味品在发酵过程中易产生多种潜在的有毒代谢物,其中生物胺是影响其质量和安全的重要风险因素之一,过量摄入会使人体产生各种毒害反应,从而对健康造成不良影响。文章对生物胺的产生原因、毒性和检测方法进行了归纳,并重点阐述了国内外关于生物胺的物理、生物和化学的防控措施,以期为酿造调味品的食用安全性及有效控制提供新思路。

白铅矿(PbCO_(3))和菱锌矿(ZnCO_(3))硫化机理的DFT研究

采用密度泛函理论(DFT)比较研究白铅矿(PbCO_(3))和菱锌矿(ZnCO_(3))硫化机理的差异。通过在PbCO_(3)/ZnCO_(3)表面构建Pb-S/Zn-S层来模拟硫化结构。层距和Mulliken电荷的结果表明,PbCO_(3)上形成稳定的Pb-S层,而ZnCO_(3)上形成的Zn-S层不稳定。由于Pb-S层具有高的共价性,而Zn-S层具有高的离子性,因此,硫化-黄药法对PbCO_(3)浮选有效,对ZnCO_(3)浮选无效。为了回收ZnCO_(3),需要强离子性捕收剂,因此,硫化-胺法在ZnCO_(3)浮选中应用较广。PbCO_(3)和ZnCO_(3)表面硫化层结构和浮选行为差异主要是由于金属离子(Pb^(2+)和Zn^(2+))和配体(O配体和S配体)极化率的不同以及Zn^(2+)3d^(10)轨道的惰性造成的。