2,2’-二甲基-1,1’-联二蒽醌合成工艺的优化

以邻苯二甲酸酐和甲苯为原料,三氯化铝为催化剂,以发烟硫酸为闭环剂,二氯乙烷为介质,闭环生成2-甲基蒽醌;在活化铜粉为催化剂,以萘为溶剂下脱氯缩合制得2,2’-二甲基-1,1’-联二蒽醌,并对合成工艺进行了优化。优化条件为:采用分步法,制取2-甲基蒽醌,以萘为溶剂,n铜粉∶n1-氯-2-甲基蒽醌=1,反应温度230℃,保温3 h,在此条件下,目标产收率比原工艺提高10%。采用熔点测定、红外光谱(IR)、液相色谱(HLPC)进行分析和结构表征。     

1,1''''-联-2-萘酚的拆分进展

综述了近几年来1,1'-联-2-萘酚的拆分研究状况,并对其今后的发展提出展望.     

球磨机中无溶剂合成1,2-双取代苯并咪唑

在球磨机中无溶剂条件下,FeCl3.6H2O催化邻苯二胺与芳香醛反应,选择性地合成了1-芳甲基-2-芳基双取代苯并咪唑,产率均在80%以上。产物结构经1HNMR、13CNMR及HRMS表征。最佳反应条件为:球磨机转速400 r/min,n(FeCl3.6H2O)∶n(邻苯二胺)∶n(芳香醛)=0.25∶1∶2,研磨时间2 h。     

磁性纳米Fe_3O_4促进的固相合成2,2’-二羟基-1,1’-联萘

研究了磁性纳米Fe3O4促进的2-萘酚氧化偶联合成2,2’-二羟基-1,1’-联萘(BINOL)的反应,反应以空气中的O2为氧化剂,无溶剂的固相条件下进行。结果表明,在优化条件下:反应温度130℃,反应时间3.5 h,n(2-萘酚)∶n(Fe3O4)=1.7∶1,BINOL的收率达到99.0%,且磁性纳米Fe3O4连续循环使用5次,BINOL的收率无明显降低。     

1,1＇-联二萘酚化合物的合成研究新进展

1,1＇-联-2-萘酚类化合物是具有C2轴不对称联芳香族化合物,已在不对称合成、分子识别、农药尤其是医药等领域有着广泛的应用。本文综述了1,1＇-联-2-萘酚类化合物的基本性能、应用以及国内外最常用与最新的合成方法。     

1,1’-联-2-萘酚拆分工艺研究

研究了用手性苯乙胺和硼酸拆分消旋联萘酚,当消旋联萘酚与手性苯乙胺之比为1∶1.5(mol)、拆分时间为12h时,可以得到收率为44%、光学收率高于99%的手性联萘酚。     

1,1′-联二萘酚的合成及其在不对称合成中的应用

1 ,1′-联二萘酚是具有 C2 -对称轴的手性原料 ,已广泛用于合成手性医药、农药、香料及食品添加剂中。较为详细地概述了 1 ,1′-联二萘酚的合成进展 ,并以其合成的手性配体为线索论述了其在不对称合成中的应用     

2,2′-联萘酚及其衍生物的合成研究进展

总结了消旋联萘酚、手性联萘酚的合成进展,以及它们在制备联萘酚衍生物中的应用进展,重点介绍了所用的氧化剂、催化剂等反应条件。指出应加强对联萘酚的合成研究,特别是高效的手性催化合成研究,和手性联萘酚衍生物的合成和应用研究。     

2,2′-二羟基-1,1′-联萘合成方法综述

综述了 2 ,2′ 二羟基 1,1′ 联萘 (联萘酚 )的合成方法 ,包括外消旋体的合成以及手性合成。参考文献 5 1篇     

两种水相中制备1,1'-联-2,2'-二萘酚的方法

介绍了两种在水相中利用2-萘酚氧化偶合制备外消旋1,1’-联-2,2’-二萘酚的催化剂,并对不同反应条件下的产率进行了研究。结果表明[Cu(NH3)4]2 作催化剂时,产率可达97%;而新制的Cu(OH)2作催化剂时,产率则达到了91%。     

2-氯乙基乙基醚的无溶剂合成

对2-氯乙基乙基醚的合成工艺进行了无溶剂合成改进。以三乙胺为催化剂，乙二醇单乙醚与二氯亚砜反应，产物经饱和碳酸钠溶液碱洗、饱和氯化钠溶液水洗、无水硫酸钠干燥，得2-氯乙基乙基醚，并采用1H-NMR和GC-MS对产物结构进行了表征。采用单因素实验研究了投料摩尔比例、反应温度和反应时间对产物色谱纯度和收率的影响。优化后，投料摩尔比例为n(乙二醇单乙醚):n(二氯亚砜):n(三乙胺)=1.0:1.3:0.3、反应温度为70 ℃、反应时间为4 h。在此工艺下经公斤级中试放大，产品的收率可达90.2%以上、色谱纯度达到99.4%以上、含量达到99.2%以上。     

Surface modification of calcite by wet-stirred ball milling and its properties

This paper investigates the surface modification of calcite from the Ni?de region of Turkey with sodium oleate (SDO) as a modification agent, which is incorporated into the calcite with wet ultra-fine grinding in a laboratory stirred ball mill. The effect of surface modification is evaluated by a floating test, which measures the active ratio (AR), fourier transform infrared spectrometry (FT/IR) and thermogravity analyses (TG-DTA). The results indicate that the hydrophilic surface of calcite becomes hydrophobic after the incorporation of SDO through wet-stirred ball milling.     

高能球磨制备超细活性SiO_2微粉工艺研究

通过研究硅藻土的结构,在传统工艺基础上提出了以硅藻土为原料.高能球磨法制备超细活性SiO2微粉的 新工艺。     

Effect of ball size and powder loading on the milling efficiency of a laboratory-scale wet ball mill

Alumina powder was wet-milled by zirconia balls with varying diameter at varying rotation speed, and the resultant particle size of the milled powder was analyzed. At a given rotation speed, there exists an optimum ball size to yield minimum particle size of alumina. The optimum ball diameter decreases as the rotation speed increases. This result has been interpreted in light of the competition between the reduced kinetic energy of the smaller balls (a negative source for milling efficiency) and the increased number of contact points of the smaller balls (a positive source), which yields the optimum ball diameter at an intermediate size. As the rotation speed increases, kinetic energy of the balls increases, which, in turn, shifts the optimum ball size toward a smaller value. As the powder loading increases from 1 to 35 g at a given rotation speed and ball size, the milling efficiency decreases monotonically.     

1-氮杂-2-甲氧基-1-环庚烯的无溶剂合成

以己内酰胺和硫酸二甲酯为原料,在无溶剂条件下合成了1-氮杂-2-甲氧基-1-环庚烯,考察了反应时间、反应温度、反应物配比等对反应收率的影响。结果表明:当反应物n(己内酰胺)∶n(硫酸二甲酯)=1∶1时,80℃反应2h,反应生成1-氮杂-2-甲氧基-1-环庚烯己内酰胺的收率72.3%。     

杂多酸催化7-羟基-4-甲基香豆素的无溶剂合成

报道了以杂多酸(H3PW12O40、H3PMo12O40、H8SiW12O42、H6P2W18O40、H4SiW12O40、H6PMo6W6O40)为催化剂,以乙酰乙酸乙酯和间苯二酚为原料,通过Pechmann反应合成标题化合物的方法。探讨了以H4SiW12O40为催化剂时反应温度、催化剂用量、反应时间、原料比诸因素对产品收率的影响。实验表明,H4SiW12O40是合成标题化合物的良好催化剂,在反应温度为130℃,反应时间为50min,n(间苯二酚)∶n(乙酰乙酸乙酯)=1∶1.3,催化剂用量为1.5%(与间苯二酚的物质的量比)时,产品收率75.9%。     

Microwave synthesis and sintering of forsterite nanopowder produced by high energy ball milling

This paper reports the development of a new process for the synthesis and sintering of forsterite nanopowder via microwave-assisted high energy ball milling of a powder mixture containing silica gel and Mg(OH)₂. X-ray diffraction (XRD), FTIR spectrometer, BET, scanning electron microscopy (SEM) and Transmission electron microscopy (TEM) techniques were utilized to characterize the as-milled and annealed samples. X-ray diffraction results showed that highly ordered forsterite can be obtained through the calcination of the as-milled powder over 900 °C. In addition, SEM and TEM observations of the synthesized powders showed that the particle size of the powder lies in the nanometer range, also being compared with the BET results (about 45 to 64.5 nm). Microwave sintering (MS) of the forsterite nanopowder produced with high energy ball milling and subsequent microwave heating resulted in remarkable enhancement in densification in comparison with conventional sintering (CS) at lower temperatures.     

Effect of processing parameters on the formation process of nano-sized ZrB2 powders by the high energy ball milling

ABSTRACT

Nano-sized ZrB₂ powders were synthesised using the high energy ball milling with ZrO₂ and B₂O₃ as raw materials and Mg as the reducing agent. The resulting powders were characterised by X-ray diffraction, scanning electron microscopy, laser particle size analysis, transmission electron microscopy, energy dispersive spectrometry, and X-ray photoelectron spectroscopy. The influence of the synthesis parameters, including the ratios of ZrO₂ to B₂O₃, milling medium, and reaction time, on the synthetic course of the ZrB₂ nanopowders were studied systematically. The mechanisms by which these parameters influence the synthetic course of and the resulting product quality are determined. Ultimately, the diameter of the resulting particles is about 200–400?nm, which are an agglomeration composed of many individual small particles with an average diameter of ～50?nm. In addition, the oxidation of ZrB₂ powders has also been studied.