苄基乙酰乙酸乙酯和丁基乙酰乙酸乙酯的微波合成

在氢氧化钾作用下,分别以乙酰乙酸乙酯和苄基氯、乙酰乙酸乙酯和1-溴丁烷为原料(摩尔比为1：1．2),180W微波辐射60s,合成苄基乙酰乙酸乙酯和丁基乙酰乙酸乙酯,此条件下两种目标产物的收率分别达71．3％和63．2％。     

室温离子液体1-丁基-3-甲基咪唑磷酸二丁酯的电导率研究

利用磷酸三丁酯与N-甲基咪唑在恒温150℃下一步合成了离子液体1-丁基-3-甲基咪唑磷酸二丁酯,考察了其在丙酮,水,DMF,乙酸溶剂中的电导率及摩尔电导率。实验发现该离子液体在不同溶剂中的电导率(κ)相差很大,其顺序为κa(水)>κb(DMF)>κc(丙酮)>κd(乙酸)。在相同温度下,电导率及摩尔电导率随浓度的增大而增大;在相同浓度下,电导率及摩尔电导率随温度的升高而增大。     

含纳米二氧化硅粒子的丙烯酯丁酯细乳化

为了调控含纳米SiO₂的丙烯酸丁酯细乳化后液滴的粒径及粒径分布,研究了细乳化体系组成和超声分散条件对细乳化液滴粒径及粒径分布的影响.发现存在使细乳化液滴粒径及粒径分布趋于稳定的临界超声功率和超声时间;随着十二烷基硫酸钠（SDS）乳化剂浓度增加,液滴粒径减小,而十六烷浓度对液滴粒径影响较小;随着BA分散液中纳米SiO₂质量分数和BA分散液/水质量比的增加,液滴平均粒径增大,粒径分布变宽,这是由于纳米SiO₂粒子吸收了部分超声波能量,同时改变了分散相特性所致.当放置或聚合温度在65℃以下时,细乳化液或相应的聚丙烯酸丁酯/纳米SiO₂复合乳胶能稳定分散.     

Poly(silyl ester)s: A new route of synthesis via the condensation of Di‐tert‐butyl ester of dicarboxylic acid with dichlorosilane

Poly(silyl ester)s were synthesized by a new route via the condensation of di‐tert‐butyl ester of dicarboxylic acid with dichlorosilane by the elimination of tert‐butyl chloride as a driving force. Three new poly(silyl ester)s with molecular weights typically ranging from 2000 to 5000 amu were produced by the condensation of di‐tert‐butyl adipate with 1,5‐dichloro‐1,1,5,5‐tetramethyl‐3,3‐diphenyl trisiloxane and di‐tert‐butyl fumarate with 1,5‐dichloro‐1,1,5,5‐tetramethyl‐3,3‐diphenyl trisiloxane or 1,3‐dichlorotetramethyl disiloxane. Each polymer was characterized with infrared, ¹H‐NMR, and ¹³C‐NMR spectroscopy, gel permeation chromatography, differential scanning calorimetry, and thermogravimetric analysis. This new approach showed several advantages. First, it did not require a catalyst or solvent. Second, the tert‐butyl chloride byproduct was volatile and was easily eliminated. Third, there was no reaction between the growing poly(silyl ester)s and the condensation byproduct, tert‐butyl chloride. Fourth, the monomers could be readily purified. Finally, the polymerization could be performed at relatively low temperatures and in a short time. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 1378–1384, 2006     

毛细管色谱法测定酸烯合成的醋酸酯产品

采用50 m×0.25 mm×0.25μm OV 101石英毛细管柱,建立了醋酸和轻烯烃直接合成的醋酸丁酯类产品色谱分析方法,并测定了醋酸仲丁酯和醋酸叔丁酯产品中常见组分的相对校正因子。采用恒温分离,在获得满意分离效果的同时降低了仪器要求。方法精密度较好。     

挤出用溴化丁基橡胶硫化体系的研究

溴化丁基橡胶几种典型硫化体系的对比实验,结果表明,用氧化锌体系硫化的溴化丁基橡胶具有良好的焦烧安全性,比较适宜于挤出用;加入促进剂HVA-2,可显著提高胶料的硫化速度和交联程度,并改善焦烧安全性;当氧化锌用量为4份,HVA-2用量为1.5份时,胶料具有较佳的综合物理性能和加工安全性。     

磺化硅胶催化合成2,4-滴丁酯

以2,4-二氯苯氧乙酸和正丁醇为原料,磺化硅胶为催化剂,催化合成除草剂2,4-二氯苯氧乙酸正丁酯(2,4-滴丁酯)。考察催化剂用量、原料配比及回流时间对反应的影响。结果表明,最佳反应条件为:催化剂用量为2,4-二氯苯氧乙酸质量的1.4%,n(正丁醇):n(2,4-二氯苯氧乙酸)=10:1,回流时间为1.0 h,2,4-二氯苯氧乙酸正丁酯的收率为98.7%。     

酶解淀粉-苯乙烯/丙烯酸丁酯接枝共聚物乳液的制备研究

采用无皂乳液聚合的方法,以过硫酸铵(APS)为引发剂,制备了酶解淀粉与苯乙烯(St)和丙烯酸丁酯(BA)的接枝共聚物。探讨了淀粉与单体配比、过硫酸铵用量、单体配比和反应温度对接枝反应的影响。结果表明,反应的优化条件为:m(淀粉)∶m(单体)=1∶3,(NH4)2S2O8的加入量为淀粉与单体总质量的0.5%,单体质量比为1∶1,反应温度为82℃,在此条件下,接枝率可达103.8%,接枝效率为37.4%,单体转化率为91.9%。红外光谱分析表明,苯乙烯和丙烯酸丁酯参与了接枝反应;SEM结果显示,接枝反应之后,淀粉形貌发生了变化,球状颗粒已经消失。     

A Study on the Effect of Butyl Methacrylate Content on Swelling and Controlled-Release Behavior of Poly (Acrylamide-co-Butyl-Methacrylate-co-Acrylic Acid) Environment-Responsive Hydrogels

Poly (acrylamide-co-butyl methacrylate-co-acrylic acid) [poly (AAm-co-BMA-co-AAc)]-based environment-sensitive hydrogels were prepared by varying the butyl methacrylate (BMA) content, in the range of 20 to 66% (wt. of the total monomer) in the hydrogel. The effect of BMA content on the swelling behavior of the hydrogels was studied by keeping the other two monomers' content constant at different pH and temperatures. The synthesized hydrogels were characterized by various techniques, and release kinetics was analyzed. The application and effect of the BMA content of these hydrogels in controlled drug release of acetaminophen and model drugs were investigated.     

丁黄药用作高硫铝土矿浮选除硫的捕收剂

采用浮选方法对我国含硫一水硬铝石型铝土矿进行脱硫,采用单因素实验研究了高硫铝土矿在浮选剂丁基钠黄药作用下反浮选除硫的工艺条件,考察了浮选剂用量、浮选时间、浮选矿浆浓度(液固质量比)、pH值及矿石粒度对浮选的影响. 结果表明,反浮选除硫的合适工艺条件为,矿浆pH 10、浮选剂用量0.16 kg/t、起泡剂20 g/t、浮选刮泡时间15 min、液固质量比10、矿石粒度0.15 mm. 在此工艺条件下,铝土矿中硫含量由2.08%降低到0.41%,符合我国氧化铝工业对矿石中硫含量的要求,Al2O3回收率达90.83%. 浮选过程基本符合一级动力学反应方程.