醇化法合成碲醇盐及其Sol-gel法制备碲酸盐薄膜

以二元醇和TeO2为反应物,通过醇化反应合成金属碲醇盐。利用FT-IR、Raman、DTA和OM测试手段研究了醇化反应过程及产物性质。结果发现,以反应活性高的乙二醇和1,2丙二醇为反应物可以合成出乙二醇碲和1,2丙二醇碲。与1,2丙二醇碲相比,乙二醇碲聚合程度相对较高,因此,其溶解性差、熔点高;而1,2丙二醇碲溶解性好、熔点低。XRD和FE-SEM分析表明,采用本实验合成的1,2丙二醇碲,通过溶胶-凝胶法可制备出适用于光电器件的碲酸盐薄膜材料。

One-pot cascade conversion of xylose to furfuryl alcohol over a bifunctional Cu/SBA-15-SO3H catalyst

The conversion of hemicellulose-derived xylose to furfuryl alcohol is a practical procedure for producing value-added chemicals from biomass.In this study,a bifunctional Cu/SBA-15-SO3 H catalyst was employed for the one-pot catalytic conversion of xylose to furfuryl alcohol with a yield of up to 62.6% at the optimized conditions of 140℃,4 MPa,and for 6 h in a biphasic water/n-butanol solvent.A high reaction temperature resulted in further hydrogenation to 2-methyl furan,while a high hydrogen pressure led to a side hydrogenation reaction to xylitol.The biphasic solvent allowed xylose solvation as well as furfuryl product extraction.The acidic-SO3 H sites and Cu sites co-existed,maintained a balance,and cooperatively catalyzed the cascade conversion.Excessive acidic sites and large pores could promote the xylose conversion,although a low furfuryl alcohol yield was obtained.This catalytic system could be potentially applied to the one-pot synthesis of furfuryl alcohol from hemicellulose-derived xylose.

Synthesis and characterization of mibolerone

A simple and effective route for the synthesis of mibolerone was described starting from the estr-5(10)-en-3,17-dione in four steps with the overall yield of 47.0 %.Thus,two methods for key intermediate methylnorandrost were investigated:one(method A)starting from estr-4-en-3,17-dione underwent 3-keto group protected with ethyl orthoformate to give 3-ethoxy-3,5-dien-estr-17-one,the other(method B)from estr-5(10)-en-3,17-dione and protected 3-keto group to give 3,3-dimethoxy-estr-5(10)-7-one in a mild acidic condition.Then,two intermediates were subsequently reacted with methyllithium followed by a mild hydrolytic procedure and gave methylnorandrost with total yield 25.0% and 86.0 %,respectively.In the preparation of 6-dehydrogenation product of methylnorandrost,two procedures(method C and method D)were investigated:one was the protected 17α-methyl-17β-hydroxy 3,5-enol ethers estrendiene brominated and the resulting 6-bromo-19-methylnortestosterone was then immediately dehydrohaloenated to give 6-dehydro-19-methylnortestosterone,the total yield only reaches 36.0%;the other was directly dehydrogenated with chloranil and the yield reaches 75.6% under the optimum conditions:in refluxing tetrahydrofuran,the molar ratio of methylnorandrost to chloranil is 0.66 and reaction time of 5 h.The titled compound and intermediates were characterized by 1H and 13C NMR,IRMS and elemental analysis.

Separation of Primary Alcohols and Saturated Alkanes from Fisher–Tropsch Synthesis Products

A method for separating primary alcohols and saturated alkanes from the products of Fisher-Tropsch synthesis is developed. The separation scheme consists of three steps： （1） the raw material is pre-separated by fractional distillation into four fractions according to normal boiling points; （2） appropriate extractants are selected to sep- arate the primary alcohols from the saturated alkanes in each fraction; （3） the extractants are recovered by azeotropic distillation and the primary alcohols in the extract phase are purified. Based on the proposed method, the total recovery rates of the primary alcohols and the saturated alkanes are 86.23% and 84.62% respectively. 2014 The Chemical Industry and Engineering Society of China, and Chemical Industry Press. All rights reserved.

Methanol from CO2 and Solar Energy A Literature Review

The project ＂SolMethCO2＂ deals with the options of an effective methanol synthesis from atmospheric or industrial CO2 sources by implementing solar energy. First part of the projects is a wide-range survey of the many different processes and sub-processes that may be involved in methanol production and of the possibilities how to make these processes available for solarization. The different fields of research were CO2 capturing, Hg/syngas-synthesis, biotechnological techniques for methanol synthesis, photocatalytical approaches and solar reactor.