部分羧甲基纤维素合成及其结构性能

采用水—有机体系合成了部分羧甲基纤维素,在规定的温度下考查了碱和醚化剂用量、反应时间及体系中含水量对取代度的影响。通过1R、X-射线衍射、DSC测试和产物特性粘数[η]的测定对其结构和性能作了表征。     

改性葡萄糖印染还原剂的制备及性能研究

以葡萄糖、戊二醛、焦亚硫酸钠为原料,通过羟甲基化和磺化反应制备出新型高效环保还原剂,优化了合成工艺,红外光谱表征了产品结构,对比了合成还原剂和保险粉的性能。通过优化实验确定了制备的最佳工艺:葡萄糖/戊二醛/焦亚硫酸钠的摩尔比为1∶3.5∶1.5、羟甲基化反应温度为70℃、羟甲基化反应时间为1.5 h、磺化反应温度为95℃、磺化反应时间为3 h,产品在30℃、还原剂质量浓度为5 g/L、NaOH质量浓度为15 g/L条件下5 min的还原电位为-933 mV。性能测试结果表明合成的还原剂在空气中保持稳定的时间以及其还原性能均优于市售的保险粉。     

碳纸负载电极在乳液法合成聚苯胺电化学性能分析中的应用

首次采用碳纸负载聚苯胺(PAn)为工作电极,探讨了反应时间对乳液法合成PAn电化学性能(循环伏安、交流阻抗及塔菲尔曲线)的影响,并通过对产物电导率、产率及特性粘度的对比分析,印证了产物电化学性能的表征结果.实验结果表明,循环伏安曲线均能有效表征出PAn的三对氧化还原特征峰,交流阻抗曲线均出现一个几乎完整的半圆;且产物的循环伏安、交流阻抗、塔菲尔、产率及电导率随反应时间的变化趋势一致,在反应5h时,PAn的各项性能指标较好.结果显示,利用碳纸作为负载电极,可以对乳液法合成PAn的电化学性能实施有效的实时表征.     

锂离子电池正极材料LiFePO_4的微波合成及结构表征

以乙酸锂、草酸亚铁、磷酸二氢铵为原料,利用微波法制备出锂离子正极材料磷酸亚铁锂,同时在不同的时间下研究其对反应物合成的影响.用X射线衍射技术、扫描电子显微镜等对产品的晶体结构进行表征,结果表明:微波合成法具有反应时间短、能耗小、合成效率高等优点,其合成的磷酸亚铁锂的晶体结晶度较好、粒度分布较均匀、晶粒比较完整;同时也证实了微波合成是一种比较好的合成方法.     

硅钨酸掺杂的聚苯胺：实物模板法制备及催化性能

以不同形态的实物为模板,硅钨酸为掺杂剂,过硫酸铵为氧化剂合成了不同微观形貌掺杂态聚苯胺,并用红外光谱、气相色-质联用仪及扫描电镜对其进行了表征。考察了所制备的聚苯胺催化合成环己酮1,2-丙二醇缩酮的性能,探讨了不同微观形貌掺杂态聚苯胺催化剂对缩酮反应的催化活性,研究了催化剂用量、反应时间等因素对产品收率的影响,以及不同沸程的产物。结果表明:硅钨酸掺杂聚苯胺是合成环己酮1,2-丙二醇缩酮的良好催化剂,其中微观结构为球状的聚苯胺催化性能最佳。在n环己酮∶n1,2-丙二醇=1∶1.4,催化剂用量为反应物总质量的1.6%,反应时间为40 min的最佳条件下,环己酮1,2-丙二醇缩酮的收率为89.2%。     

锂离子电池正极材料LiFePO4的微波合成及结构表征

以乙酸锂、草酸亚铁、磷酸二氢铵为原料,利用微波法制备出锂离子正极材料磷酸亚铁锂,同时在不同的时间下研究其对反应物合成的影响.用X射线衍射技术、扫描电子显微镜等对产品的晶体结构进行表征,结果表明：微波合成法具有反应时间短、能耗小、合成效率高等优点,其合成的磷酸亚铁锂的晶体结晶度较好、粒度分布较均匀、晶粒比较完整;同时也证实了微波合成是一种比较好的合成方法.     

离子液体热合成磷仲钨酸铯杂多酸盐催化环己醇制备环己酮

采用离子液体热合成法合成新型磷仲钨酸铯杂多酸盐Cs_3PW_(12)0_(40)’系列催化剂并对其物化性能进行了表征.同时以Cs_3PW_(12)0_(40)’-80(简称CsPW’-80)为催化剂, 30%H_2O_2为氧化剂,乙腈为溶剂,以氧化环己醇合成环己酮为催化剂性能测试反应进行催化性能评估.考察了合成催化剂溶剂离子液体占比、催化剂用量、氧化剂用量、反应温度以及反应时间对催化性能的影响.实验结果表明:在合成催化剂离子液体占比为80%、乙腈溶剂5 mL、氧化剂与反应物n(30%H_2O_2)/n(cyclohexanol)=4、反应温度70℃、反应时间8 h的最优条件下,环己醇转化率为100%,环己酮的选择性为98.46%,环己酮总收率达到98.46%.     

酸功能化离子液体催化合成柠檬酸三丁酯

合成并表征了酸功能化离子液体,用于催化合成柠檬酸三丁酯(TBC).通过考察各种离子液体的催化活性及重复使用性能,选定酸功能化离子液体[HSO3-pmim]HSO4为催化合成TBC的催化剂.研究了催化剂用量、醇酸摩尔比、反应时间等因素对酯化反应的影响,得到其较佳工艺条件为:催化剂用量为反应物总质量的8·0%,醇酸摩尔比为5·5∶1,反应温度110~150℃,反应时间3h.此条件下,酯化率达到99·0%.分离出的离子液体未经任何处理重复使用8次后,酯化率仍为95·2%.     

BiOBr的制备及其光催化性能的研究

以氧化铋为原料,采用水解法合成了溴氧化铋光催化剂,采用X射线衍射仪对溴氧化铋晶体进行表征,研究了溴氧化铋晶体降解罗丹明B溶液的光催化性能。实验结果表明,在反应温度为40℃、反应时间为90 min合成的Bi OBr光催化性能最好,具有较强的光催化活性,其催化活性优于Bi OCl催化剂,其催化降解罗丹明B反应表现为假一级动力学。     

新型甲基吲哚季铵盐的制备及其光电性能研究

以2,3,3-三甲基吲哚为原料,合成了5种甲基吲哚阳离子季铵盐,通过核磁共振氢谱、质谱等手段,对合成的化合物进行了结构表征,并将其作为有机电解质应用于染料敏化太阳能电池,测定了其相应的光电转换效率,探讨了阳离子季铵盐化合物结构与光电性能的关系.     

Structure of the first silicate molecular sieve with 18-ring pore openings, ECR-34

The three-dimensional microporosity of zeolite frameworks have allowed their widespread use in industry as heterogeneous catalysts, absorbents, and ion-exchangers. While the phosphate analogues of zeolites having up to 24 tetrahedral atoms in the pore openings are known, silicate-based zeolites have, until now, been limited to 14-membered ring pore openings. We now disclose the structure and characterization of the synthetic zeolite ECR-34, which can be prepared from a mixed alkali metal reaction gel containing tetraethylammonium (TEA) cations. Its structure has been determined from powder diffraction data and shows ECR-34 to be hexagonal with the dimensions a, b = 21.030(1) A, c = 8.530(1) A, containing one-dimensional, 18-ring pores with 10 A diameter free openings. ECR-34 is stable to 800 degrees C and is able to absorb and ion-exchange large organic molecules. The existence of ECR-34 suggests the potential of preparing other thermally stable silicate molecular sieves with extra-large pores.     

Y沸石水热转晶为ECR-1沸石的研究

ECR-1具有十二元孔道, 其通常是在有机模板存在下合成的, 我们曾报道了在无有机模板剂的条件下合成沸石ECR-1, 本文报道在无有机模板剂存在的条件下Y沸石水热转晶为沸石ECR-1的研究结果. 因为Y沸石具有合成简单、价格低廉和不使用有机模板等特点, 所以对由Y沸石转晶为ECR-1的研究, 对其在工业上的应用具有重要意义.     

Evaluation of phase transformation behaviors of zeolite and antibacterial properties against Gram-positive and -negative bacteria

This study deals with the synthesis of zeolite from natural kaolinite using hydrothermal treatment and evaluation of its phase transformation behaviors. The synthesized zeolites were modified with silver ion by using the ion exchange method for the enhancement of antibacterial properties. The characterizations were performed by using X-ray diffraction spectroscopy, Fourier-transform infrared spectroscopy, field emission scanning electron microscopy, and energy-dispersive X-ray. Disk diffusion technique (DDT) was used for the evaluation of the antibacterial property of the modified zeolites. This study observed the transformation of kaolinite into amorphous metakaolin after calcination treatment at 900°C and the successful reconstruction of amorphous metakaolin into synthesized crystal zeolite in the presence of sodium hydroxide as an activating agent. It was also found that the zeolite type A was produced at 100°C, while sodalites were produced at 120 and 140°C. DDT analysis revealed that the modified zeolites showed significant antibacterial capability against Escherichia coli ATCC 11229 and Staphylococcus aureus ATCC 6538. In general, the present study has proven that the zeolites can be synthesized from natural material and can be modified with silver ion to enhance their antibacterial activity.     

高温合成NaY沸石

提出了应用NaY沸石导向剂提供全部硅源合成NaY沸石的新方法, 研究了高温条件下合成NaY沸石的规律和特点, 发现在高温条件下合成NaY沸石不仅晶化速度快, 而且可以在不加有机物的条件下合成较高硅铝比[n(SiO2)/n(Al2O3)=6]的NaY沸石.     

A working hypothesis for broadening framework types of zeolites in seed-assisted synthesis without organic structure-directing agent

Recent research has demonstrated a new synthesis route to useful zeolites such as beta, RUB-13, and ZSM-12 via seed-assisted, organic structure-directing agent (OSDA)-free synthesis, although it had been believed that these zeolites could be essentially synthesized with OSDAs. These zeolites are obtained by adding seeds to the gels that otherwise yield other zeolites; however, the underlying crystallization mechanism has not been fully understood yet. Without any strategy, it is unavoidable to employ a trial-and-error procedure for broadening zeolite types by using this synthesis method. In this study, the effect of zeolite seeds with different framework structures is investigated to understand the crystallization mechanism of zeolites obtained by the seed-assisted, OSDA-free synthesis method. It has been found that the key factor in the successful synthesis of zeolites in the absence of OSDA is the common composite building unit contained both in the seeds and in the zeolite obtained from the gel after heating without seeds. A new working hypothesis for broadening zeolite types by the seed-assisted synthesis without OSDA is proposed on the basis of the findings of the common composite building units in zeolites. This hypothesis enables us to design the synthesis condition of target zeolites. The validity of the hypothesis is experimentally tested and verified by synthesizing several zeolites including ECR-18 in K-aluminosilicate system.     

A Study of the Encapsulation of Nickel Phthalocyanine in Molecular Sieve Zeolites of the FAU Type

Nickel(II)phthalocyaninate spectroscopy (NiPc) was synthesized in the supercages of zeolite FAU by the template synthesis method at two different temperatures of 200 and 300°C and characterized by diffuse reflectance spectroscopy, UV-Vis spectroscopy, X-ray powder diffraction, and IR. The results show that the catalyst synthesized at 200°C contains a higher amount of complex as monomeric species encapsulated in the supercages. At elevated temperature, higher amount of the NiPc may be hosted in the mesopores and/or on the external surface of the zeolite as aggregates.     

Pulsed laser ablated zeolite nanoparticles: A novel nano-catalyst for the synthesis of 1,8-dioxo-octahydroxanthene and N-aryl-1,8-dioxodecahydroacridine with molecular docking validation

There is an increasing interest in the synthesis of metal nanoparticles (NPs) from bulk metals using pulsed laser ablation in liquids (PLAL), as it offers an easy and simple synthesis route. In this work, zeolite NPs (molecular sieve 4A) were successfully synthesized by the PLAL technique, and characterized by X-ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, transmission electron microscopy, field emission scanning electron microscopy, and high-resolution transmission electron microscopy. Data obtained confirm the formation of the crystalline phase of zeolite. The synthesized catalyst (zeolite molecular sieve 4A) was used as an efficient and facile promotor for the synthesis of xanthene and acridine derivatives. Molecular docking of the synthesized compounds was validated using quinone reductase 2 (NQO2) and acridine orange as the ligand, with the synthesized molecules showing good drug–ligand interaction on the active site of NQO2, compared with that of acridine orange.     

The Influence of the Synthesis Temperature on Cobalt Phthalocyanine Encapsulation in Zeolite Y

Several characterization techniques were applied to study the effect of the synthesis temperature on the physicochemical properties of cobalt phthalocyanine incoporated into zeolite Y. The cobalt phthalocyanine was synthesized in the supercages of zeolite Y by the template synthesis method at two different temperatures of 200 and300 °C and characterized by diffuse reflectance spectroscopy, Fourier transform infraredspectroscopy, pore volume analysis, unit cell dimension calculation, UV-vis spectroscopy,thermogravimetric analysis and X-ray diffraction. The results show that the catalyst synthesizedat 200 °C contains 11 wt.% cobalt phthalocyanine and almost all of thiscomplex is encapsulated in the supercages as monomeric species. At higher temperature aconsiderable amount of the cobalt phthalocyanine is hosted in the mesopores and/or on theexternal surface of the zeolite as aggregates. The migration of one part of the cobalt cationsfrom the supercages to the small cages at 300 °C decreases the formation of thenon-aggregated encapsulated phthalocyanine molecules in the zeolite supercages. Theaggregated cobalt phthalocyanine formed at the surface corresponds to the -polymorph stateof the phthalocyanine.     

Framework‐Substituted Bismuth Zeolite‐P: Synthesis and Characterization

Bismuth‐modified zeolite‐P (Bi‐ZP) was synthesized by hydrothermal methods during the phase transformation of analcime to zeolite‐P. The evolution of phase transformation of pure analcime to Bi‐ZP was investigated. The results showed that bismuth atoms were incorporated into the framework of the microporous zeolite‐P. The effect of various Bi/Al (0–3) and Si/Bi (1–5) mole ratios on the synthesis of bismuth modified zeolite were studied by X‐ray diffraction (XRD) technique and FT‐IR spectroscopy. Evolution of the growth process of Bi‐ZP spheres was carried out at different time intervals with XRD patterns and FE‐SEM images. The energy dispersive X‐ray (EDX) spectrum indicated the existence of bismuth atoms in the synthesized Bi‐ZP. Framework substitutions of bismuth were evidenced by a set of complementary characterizations such as diffusive reflectance UV/Vis (DRS) and Raman spectroscopy on the synthesized Bi‐ZP (Si/Bi = 1).     

Y沸石的高温合成

采用甲基三乙氧基硅烷(MTS)为添加剂, 在高温(140 °C)条件下水热合成出具有六方片状形貌的Y型沸石. 相比于100 °C左右合成的Y型沸石, 高温合成的Y沸石具有更高的硅铝比值、更大的晶体宽厚比值以及对有机挥发物具有优异的吸附性能. 通过X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、²⁹Si固体核磁共振(NMR)、傅里叶变换红外(FTIR)光谱、碳氢氮元素分析(CHN)、水接触角等表征, 证明了所合成的新型Y沸石具有甲基基团, 它们的存在增强了疏水性能, 提高了对有机挥发物的吸附能力.