固体酸SO4(2-)/Nb2O5催化合成尼龙酸二异丁酯

研究了SO4^2-／Nb2O5作为催化剂催化合成尼龙酸二异丁酯的反应。通过正交试验确定了最佳反应条件：酸醇物质的量比为1：2．5，催化剂为反应物总量的0.35％，反应回流2．0h，在此条件下酯化率可达97．8％。     

A Comparison of the Migration of ‘Spiked’ and ‘Intrinsic’ Substances from Paper and Board into Raisins and into Tenax as a Food Simulant

Four samples of paper and board (P/B) of a type used for packaging dry foods were subjected to migration experiments using raisins and the polymeric powder Tenax as a food simulant. The P/B samples contained only low levels of diisopropylnaphthalene (DiPN) and diisobutyl phthalate (DiBP), and so, experiments were also conducted after spiking the P/B with added model substances. These were o‐xylene, acetophenone, dodecane, benzophenone, DiPN and DiBP. Migration experiments into raisins and Tenax were conducted for 10 days at 40°C. Migration levels depended strongly on the nature of the substance. Migration from spiked P/B samples was more extensive (as a percentage of that available) than migration of intrinsic migratable substances, and so, studying spiked samples tends to be conservative. It is considered likely that this is because of binding of substances, especially aromatics with pi‐electrons such as DiPN and DiBP, to active sites on the surface of P/B fibres, resulting in non‐linear absorption isotherms. However, further work would be needed to prove this conclusively. Considering the results overall and also that raisins packed in P/B can have a shelf life of up to 1 year at ambient temperatures, the test results using Tenax as a food simulant are considered to be appropriate without application of a correction factor. Copyright © 2014 John Wiley & Sons, Ltd.     

DIBK-TBP体系萃取分离锆铪的机理

为了解二异丁基甲酮(DIBK)-TBP体系萃取锆铪的化学行为,分别采用斜率法和饱和容量法研究DIBK和TBP在HSCN介质中协同萃取锆铪的性能及机理,结果表明:DIBK-TBP体系萃取分离锆铪时优先萃取铪,萃取反应机理为溶剂化机理,萃合物中Zr4+(Hf4+)、TBP、DIBK的摩尔比为1:1:1,其萃合物组成分别为Zr(SCN)4.TBP.DIBK和Hf(SCN)4.TBP.DIBK,并通过对负载有机相进行红外光谱分析进一步确定了萃合物可能的结构式;DIBK和TBP协同使用可以改善HSCN介质下锆铪的萃取分离效果。     

环己基甲基二甲氧基硅烷的合成

将环己醇氯化，生成的氯代环己烷制成格氏试剂，使之与甲基三甲氧基硅烷反应。反应产物经精制即为高纯度产品。     

苯酐渣制备邻苯二甲酸二异丁酯增塑剂

苯酐渣系萘氧化或邻二甲苯氧化的副产物。在杂多酸催化下 ,与异丁醇直接酯化再经减压蒸馏制得合格的邻苯二甲酸二异丁酯 (DIBP)增塑剂 ,苯酐回收利用率可达 95 %以上。在 30 0t/aDIBP工业生产装置上 ,考察了催化剂用量、原料配比、反应温度和时间、搅拌及蒸馏压力等因素对制备产品的影响。其最佳工艺条件为 :(1)酯化反应 :催化剂用量为反应物总质量的1 0 % ,n(异丁醇 )∶n(苯酐 ) =1 2∶1 0 ,温度 12 0～ 16 0℃ ,时间 4h ,反应在搅拌下进行 ;(2 )减压蒸馏 :蒸馏压力≤ 5 0kPa。     

N-β(氨乙基)-γ(氨丙基)甲基二甲氧基硅烷的合成与生产

介绍以国产原料、采用氯铂酸复合催化剂进行硅氢加成，醇解和胺化反应，合成氨乙基氨丙基甲基二甲氧基硅烷，实现工业化生产，并在许多行业中得到广泛应用。讨论了工艺过程对产品性能、收率的影响因素。     

DIBK溶剂萃取法分离锆铪

以二异丁基甲酮(DIBK)作萃取剂,以TBP或P204作改质剂,从不同酸性介质中萃取分离锆铪。考察酸性介质、TBP加入量、P204加入量和盐析剂(NH4)2SO4等对萃取分离锆铪效果的影响。结果表明:DIBK只有在HSCN介质中优先萃取铪,改质剂TBP或P204的加入能显著增加铪的萃取率和锆铪的分离系数。锆铪的分离系数可达到9,与MIBK萃取分离锆铪的性能相似。     

二羧酸二异丁酯的合成

以二羧酸和异丁醇为原料，用硫酸作催化剂，合成二羧酸二异丁酯。考察了醇酸质量比、反应温度、反应时间、催化剂用量等反应条件对酯化反应的影响，在大量实验基础上，确定了制取二羧酸二异丁酯工艺条件。     

耐寒增塑剂尼龙酸二异丁酯的合成研究

尼龙酸在质子酸催化下,与异丁醇直接酯化,减压蒸馏制得合格的尼龙酸二异丁酯。研究催化剂用量、反应原料配比,反应温度和时间及蒸馏压力等因素对其制备产品的影响。其最佳的工艺条件为①酯化反应:催化剂用量为反应物总质量的0.35%;n(异丁醇)∶n(尼龙酸)=2.5∶1;在搅拌条件下,反应温度控制在145～155℃,反应时间4.0 h;②减压蒸馏:蒸馏压力≤5.0 kPa。     

二羧酸和异丁醇制备尼龙酸二异丁酯

在对甲苯磺酸（VISA）催化剂的作用下,以二羧酸与异丁醇为原料制备尼龙酸二异丁酯,生产成本低,产品色泽好。确定了最佳合成条件：催化剂占总酸量的1．85％,碱用量是总酸量的3倍,塔顶温度控制在120℃时,产品指标满足醇含量小于0．20％,产品色泽好,且收率较高,能达到90％。