β-环糊精(β-CD)环的两端和外部为亲水性,而其内腔为疏水性,能与许多有机、无机和生物分子等分子形成主-客体包合物.环糊精的化学性质很稳定,一般食品中的pH不会导致环糊精的分解,环糊精溶于水后仍能保持环状结构及形成络合物的能力.β-CD作为超分子化合物主体,在生成包合物后可以改善客体分子的物理化学性质和生物活性,比如溶解度、稳定性及其生物利用度等.因此在超分子领域得到了广泛的应用.本文通过实验制备了黄连素的β-环糊精包合物.实验结果表明:黄连素用量为0.03g,β-环糊精2.0g,包合时间90 min,包合物的包合效果较好.包合物分别用紫外分光光度计、红外、粉末衍射、电子显微镜等进行测定.

席夫碱化合物具有多功能性,与中心原子形成配位形成金属配合物,使得它成为近代科学研究的热点.本文主要介绍以黄连素为原料,经Vilsmeier-Haak试剂(DMF/POCl3)甲酰化,最后分别与水合肼、盐酸羟胺反应,生成黄连素席夫碱.本文探讨了黄连素甲酰化的最佳反应条件,中间体和产物分别用UV、IR进行了表征.

以乙酰丙酮为原料,采用一锅法顺利地合成中间体4-氨基-3,5-二甲基吡唑,然后分别与系列羧酸酯反应,最终得到系列化合物N-(3,5-二甲基-1H-4-吡唑基)酰胺类化合物,最终产物进行了UV、IR、和NMR表征.

本文报道从2,6-二甲基吡啶为原料合成2,6-双苯甲酰乙酰基吡啶的经济可行的合成方法.尤其是最终的β-二酮是以反应物的物质的量的比为1:4条件下进行反应,即2,6-吡啶二甲酸二甲酯:苯乙酮=1:4时,取得产率76.2%.产品经过IR和UV的表征.

Carboxymethyl cellulose (CMC) is a kind of anion and aliphatic and water-soluble cellulose ether. It has been widely used in food, medicine, detergent etc because it has good performance in thickening, dispersion and suspension and so on. It is vividly regarded as the “Monosodium glutamate” in industry. In recent years, the CMC demand is stably growing. Improving quality and developing special type of CMC for specific user are becoming the development directions of CMC. Sugarcane bagasse (SCB), a kind of waste in the process of sugar extraction, is abundant and low-cost lignocelullosic material. SCB is mainly composed of cellulose, hemicellulose and lignin. Cellulose forms microfibril by intramolecular and intermolecular hydrogen bond, and hemicellulose and lignin are filling and adhering agent among the microfibril. Because of the special structure of SCB, chemical agents are difficult to penetrate and diffuse in it, which limits its application. Therefore, it is necessary to pretreat SCB to remove lignin and hemicellulose, reducing cellulose’s crystallinity. To utilize SCB and prepare CMC with high degree of substitution (DS), SCB was mechanically activated by a stirring-type ball mill. Using monochloroacetate (MCA) as etherifying agent and sodium hydroxide (NaOH) as catalyst, CMC was synthesized from SCB with different activation time. The effects of mechanical activation time, reaction time, reaction temperature, solid-liquid ratio, NaOH-MCA molar ratio and water content on carboxymethylation of SCB were investigated respectively by using the DS of CMC as evaluating parameter. The structure of CMC from SCB was characterized by using Fourier transform infrared spectroscopy (FTIR),X-ray diffraction (XRD) and 1HNMR spectroscopy (1HNMR). The results indicated that mechanical activation considerably enhanced the carboxymethylation of SCB, the mechanically activated SCB was easier for carboxymethylation than the original SCB, and the DS increased first and then decreased with activation time. The reasons were that mechanical activation broke the sealing of cellulose by lignin, destroyed the crystalline structure and decreased the crystallinity of cellulose, which made etherification reagent more easily penetrate into the SCB and could increase reactivity and decrease the dependence on solid-liquid ratio, ratio of NaOH/MCA, H2O/substrate, reaction time and reaction temperature. The DS and viscosity of CMC obtained were 1.521 and 13 mPa.s respectively through carboxymethylation under the conditions which were reaction time of 2.0 h, solid-liquid ratio (mass/volume) of 1:18 g/mL, NaOH-MCA molar ratio of 2:1, H2O/substrate (volume/mass) of 1:1 mL/g and reaction temperature of 75℃. The research results would provide the reference for the preparation of CMC with high DS.

刘绍荣教授，湖北石首人，1982年7月，毕业于华中师范大学化学系，同年考取中科院原子能研究所研究生，1985年7月获仪器分析专业硕士学位；毕业后留所工作；1991年出国深造。1995年7月，在美国德克萨斯州立理工大学获分析化学博士学位（导师：普南杜教授）；1996年3月至1997年3月，在美国波斯顿东北大学巴奈特研究所从事博士后研究（导师：巴里?L?卡尔格）；1997年3月-1998年3月，美国伯克利加利福尼亚大学化学系从事博士后研究（导师：里查?A?马蒂斯）；2001年12月，在美国旧金山加利福尼亚金门大学获企业管理工商硕士学位。2002年1月至现在，浙江大学客座教授。2002年1月-2007年8月，在德州理工大学化学与生物化学系任副教授，2007年9月-2007年12月任终身教授。2008年1月至今，武汉大学客座教授。2008年1月至今，任美国奥克拉荷马州马格罗里基金会会长。2008年1月至今，任美国奥克拉荷马州诺曼奥克拉荷马大学化学与生物学系终身教授。2013年10月至今，任美国奥克拉荷马州诺曼奥克拉荷马大学化学与生物学系生物分析中心主任。2014年2月-2014年6月，任澳大利亚墨尔本大学理学院名誉教授。

The cassava starch acetate of low degree of substitution were preparation using mechanical activated cassava starch which was mechanical activated for half an hour and the native starch as material acetic anhydride as acetylation reagent and sodium hydroxide as catalyst. The effects of reaction temperature, the reaction time, acetic anhydride amount and pH value on esterification of cassava starch were investigated respectively by using degree of substitution (DS) and reaction efficiency (RE)of starch acetate as evaluating parameter. The results showed that reaction temperature, the reaction time, acetic anhydride amount and pH value had certain effect on the DS and the RE of starch acetate. Mechanical activation can significantly increase the DS and the RE of starch acetate. The optimal technical conditions were obtained as reaction temperature 30℃, reaction time 40 minutes, acetic anhydride amount 0.15 mL, pH value 8.5. Under the conditions, the DS in the products was 0.075, and the RE was 87.45 %. Furthermore, the structure of activated starch and the starch acetate were further characterized by using FTIR.

无机功能材料是材料化学专业课程体系中的专业课程.课程建设中结合卓越工程师培养计划,优化教学内容,采用多种教学方法,强化实践教学,改革课程考核方式,培养高素质材料化学应用型卓越工程师.

Using Bi(NO3)3·5H2O and NH4VO3as raw materials,photocatalyst BiVO4and TiO2/BiVO4were synthesized by hydrothermal method,and characterized by X-ray diffraction(XRD),scanning electron microscope(SEM),UV-Vis techniques and infrared spectroscopy(IR).The XRD result indicated that the as-synthesized belonged to monoclinic crystal system BiVO4and after compounding with TiO2the characteristic diffraction peaks were narrowed while the intensity increased.The SEM images displayed that BiVO4were presented regular multilateral cube morphology,TiO2/BiVO4as-prepared had regular globular structure system.UV-Vis absorption spectrum indicated that BiVO4and TiO2/BiVO4responsed to visible light 400-700nm region.Based on the properties of optical absorption,selecting methylene blue as a model pollutant,the photocatalytic activity of samples were investigated.The results showed that TiO2/BiVO4had a better visible light photocatalytic activity than that of pure BiVO4,the degradation rate of methylene blue reached 95.9%.

In order to develop a new preparation method of starch acetate,the cassava starch acetate was synthesized by mechanical activation-strengthened solid phase chemical reaction.The effects of acetic anhydride content,sodium hydroxide content,ball-milling temperature,ball-milling time,stirring speed and the volume of the stack for ball-milling media on esterification of cassava starch were investigated.The degree of substitution(DS) of starch acetate was used as the evaluating parameter.The best conditions of preparation technique were confirmed by orthogonal test.The optimum conditions of cassava starch acetate preparation were 60% acetic anhydride,2.0% sodium hydroxide,ball-milling temperature 60℃,ball-milling time 60min,stirring speed 380r / min,tack media 500 mL,the DS of the products 0.2632,and the RE was 25.57%.Furthermore,the structure of native starch and the starch acetate were further characterized by using Fourier transform infrared spectrometry(FTIR) and X-ray diffraction(XRD).The mechanical activation considerably enhanced the esterification of cassava starch.

This paper discusses the pericyclic Reaction by the molecular conservation of orbital symmetry principle and frontier orbital symmetry theory.Method for predicting the possibility of pericyclic reaction and the configuration of the product under the conditions of heating and illuminating has been proposed.This method is easy to be understand and acceptable for students.

A new one-dimensional [CuC16H18N4O4S]n(1) was synthesized by the self-assembly of a ligand 2,5-thiophenediformates, 3,5-dimethylpyrazole and copper(II), and characterized by elemental analysis, IR and single-crystal X-ray diffraction. 1 crystallizes in monoclinic, space group C2/c with unit cell parameters, a=18.6156(4), b=5.96110(10), c= 18.1598(4)Å, =115.467(2)°, Z=4, V=1819.37(7)Å3, Mr = 425.94, Dc = 1.555g/cm3, μ=1.345mm-1, and F(000)= 876. The final R and wR are 0.0328 and 0.0816 for 7611 observed reflections with I>2σ(I). 1 shows an infinite 1-D polymeric chain structure based on the repeated basic units Cu(II)(3,5-dimethylpyrazole)2(2,5-thiophene diformate). The Cu(II)center acts as the joint of the unit, and is coordinated in a slightly distorted octahedral geometry comprised of four O atoms from two different 2,5-thiophenediformate ligands and two N atoms of two trans 3,5-dimethylpyrazole ligands.

Cross-linking and esterifying starch of mechanical activated maize starch was prepared by mechanical activated maize starch as raw material,and sodium trimetaphosophate as cross-linking agent and acetic anhydride in acetification.The effects of reaction temperature,cross-linking agent and esterifying agent dosage,pH value and cross-linking time on the cold viscosity of cross-linking and esterifying starch paste were investigated.The physical and chemical parameters of the cross-linking and esterifying starch of mechanical activated maize starch and cross-linking and esterifying starch of raw maize starch were studied.The structure of cross-linking and esterifying of mechanical activated maize starch were characterized by using Fourier transform infrared spectrogram(FTIR) and X-ray diffraction(XRD).The results indicated that the reaction conditions affected the preparation of cross-linking and esterifying mechanical activated maize starch.Under reaction temperature 40℃,1.0% amounts of natrium trimetpahophate,crosslinking pH at 10.0,crosslinking time 2.0 h,0.5 mL acetic anhydride amount,esterifying pH value 9.0,esterifying time 60 min,the cold viscosity of cross-linking and esterifying starch paste was enhanced from 446 mpa.s to 1 629 mPa·s.The stability,acidity-resistance,staling resistance of the viscosity of cross-linking and esterifying starch paste were significantly improved.FTIR and XRD spectra indicated that after dual-modification treatment,new chemical group was introduced,and type crystal starch was formed.

采用纳米固体超强酸SO42-/Fe2O3为催化剂,以苯乙酮和乙二醇为原料催化合成苯乙酮环乙二缩酮.优化了催化剂制备和反应条件,较适宜反应条件为:苯乙酮170 mmol,n(酮)∶n(醇)=1∶1.7,催化剂用量100 mg(占反应物总质量4.4％),(98～112)℃回流反应1.5h,苯乙酮环乙二缩酮收率达94.2％.

A Cu(II) complex of tetra(3,5-diphenyl pyrazole) [Cu(C(15)H(12)N(2))(2)Cl(2)](2) (1) was syn-thesized, and its structure was determined by single-crystal X-ray diffraction and further characterized by elemental analysis, NMR and IR. 1 belongs to the monoclinic system, space group P2(1)/c with a = 13.3780(5), b = 15.1392(6), c = 15.5923(6) angstrom, beta = 124.522(2)degrees, Z = 2 and V = 2601.86(17) angstrom(3). In 1, each Cu(2+) ion is coordinated with two N atoms from two tetra(3,5-diphenyl pyrazole) ligands and three Cl(-) anions to give a distorted square-pyramidal geometry, which is further linked through edge-sharing bridging by Cl(-) anions to form a centrosymmetric dinuclear structure.

The key intermediate,2,6-pyridinebiformyl hydrazine(3),was synthesized from 2,6-dimethyl pyridine.Six novel Schiff bases(1a～1f) in yields of 50%～97% were prepared by the reaction of 3 with aldehydes or ketones,respectively.The structures were characterized by UV,NMR,IR and MS.The preliminary antibacterial tests showed that 1 exhibited antibacterial activity to staphylococcus aureus,proteus,colibacillus and bacillus,1d was the best of all.

The adsorption and desorption properties of strong base anion exchange resin for picric acid were investigated,and the adsorption thermodynamics,kinetics and mechanism were also studied.The experimental results show that: The adsorption quantity of picric acid is increasing with the increase of adsorption temperature;When the solution pH is 2.7-12.0,the adsorption quantity is the maximum with above 120 mg/g;The adsorption isotherm of picric acid on resin accords with Freundlich model and the correlation coefficient is over 0.94;the adsorption kinetics can be characterized by Lagergren pseudo-second-order rate equation,and the activation energy of adsorption is 23.3 kJ/mol;Intraparticle diffusion is the main controlling process of the adsorption rate;The higher the initial mass concentration of picric acid is,the sooner the adsorption saturation occurs;The picric acid adsorbed on the resin can be eluted completely by the mixed solution with 2.0 mol/L HNO3 and 40%(volume fraction) acetone.

A novel mixed-ligand Zn(Ⅱ) complex(1) with 2,6-pyridinediformicacids and bis(3,5-dimethyl pyrazole) was synthesized.The structure was characterized by 1H NMR,IR,elemental analysis and X-ray single crystal diffraction.1 belongs to monoclinic,a space group C2/c with a=13.976(5),b=9.541(3),c=14.238(7),α=90.000°,β=111.386(3)°,γ=90.000°,Z=4,V=1 767.8(12) 3,Dc=1.588 g·cm-3,μ=1.424 mm-1,F(000)=872.The summit value and minimum of difference of electron density were 293 e·nm-3 and-279 e·nm-3,respectively.

In order to improve properties of starch-based biodegradable plastic films, the mechanical activated starch acetate (MASA) was synthesized from mechanical activated maize starch (MAS) with activation time for 1.0 h. At the same time, the biodegradable plastic films were produced by thermal gelatinization of starch suspensions blending MASA with degree of substitution and polyvinyl alcohol (PVA). By Fourier transform infrared spectrogram (FTIR), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM), the microstructure, particle shape, thermal stability were studied. The mechanical properties and biodegrade ability of the MASA/PVA were investigated by comparing with those of native starch acetate (SA). The results indicated that the microstructure and particle shape changed greatly and thermal property of MASA increased compared with those of MAS and native starch. The properties of MASA/PVA were better than those of SA/PVA, and the tensile strength of the MASA/PVA with MASA (DS=0.1) was 3.56 MPa, the breaking elongation was 146.22% before soaking in water, and the absorption of water was 134.79% after 24 h. Hot water resistance properties was good, and the rate of biodegradation was 45.90% in the soil after 20 days. The mechanical activation pretreatment effectively improved the properties of biodegradable plastic films.