二甲基二烯丙基氯化铵中烯丙基类杂质形成机理初探摘要本文研究了二甲基二烯丙基氯化铵（DMDAAC）单体溶液中烯丙基类杂质的形成条件，并对形成机理作了初步解释。在已有文献基础上，建立了气相色谱法用于单体中烯丙基类杂质的分析，而后对单体合成用原料、不同条件（pH、反应温度、反应时间）下单体分解破坏、常规和极端条件下单体合成工艺过程中的烯丙基类杂质进行分析检测。结果表明，对于氯丙烯、烯丙醇、烯丙醛等烯丙基类杂质，该分析方法分别在2～100mg/L范围内呈线性相关，相关系数R2分别为0.9993、0.9988、0.9997，精密度分别为1.10%～3.24%、3.40%～5.29%、1.21%～6.38%，加标回收率分别为91%～112%、97%～112%、95%～120%。DMDAAC单体破坏分解方面，随着体系pH、反应时间、反应温度的增加，杂质生成量逐渐变大。DMDAAC单体合成工艺过程方面，反应体系在高温等极端条件的烯丙基类杂质生成量明显高于常规条件下的甲醛生成量。烯丙基类杂质的形成一方面是由于氯丙烯在碱性条件下的水解以及进一步氧化，另一方面可能是由于季铵盐DMDAAC在碱性条件下形成季铵碱，进一步分解所致。在工业生产中，为避免杂质的形成，应控制DMDAAC合成反应体系始终保持低pH、低温的状态。27654
关键词 二甲基二烯丙基氯化铵 杂质 烯丙基类 机理
毕业论文设计说明书外文摘要
Title Preliminary research on the formation mechanism of allyic impurities in dimethyldiallyl ammonium chloride
Abstract
The conditions for the formation of allylic impurities in dimethyldiallylammonium chloride (DMDAAC) were researched and the formation mechanism was discussed in this paper. The gas chromatograph method for determination of allylic impurities was established based on references and present research. The allylic impurities in raw materials, decomposition at different conditions(pH, reaction temperature, reaction time) and synthesis with conventional and extreme conditions were detected. The results showed that, the linear detection ranges for allyl chloride, allyl alcohol and acrylaldehyde were 1~100mg/L, 4~100mg/L and 1~100mg/L, respectively with correlation coefficient of 0.9993, 0.9988 and 0.9997 while the recovery rate were 91%～112%, 97%～112% and 95%～120%. In DMDAAC decomposition, the amounts of allylic impurities became larger with the increase of pH, reaction time and reaction temperature. In DMDAAC synthesis, the amount of allylic impurities under extreme conditions was larger than that of normal conditions. As for the mechanism, the allylic impurities formation might be due to the hydrolysis of allyl chloride and the decomposition of quaternary ammonium alkali coming from quaternary ammonium alkaline conditions. In industrial production, low pH and low temperature should be maitained in order to avoid the formation of allylic impurities.
Keywords Dimethyldiallylammonium chloride Impurity Allylic compound Mechnism
目 录
1 引言 1
1.1 DMDAAC的性质与应用 1
1.2 DMDAAC的合成 1
1.3 DMDAAC中的杂质影响研究 3
1.4 烯丙基类杂质的研究 4
1.5 存在问题及解决思路 5
1.6 本文研究内容 5
2 实验原理 6
2.1 色谱分析原理 6
2.2 烯丙基类杂质形成原理 6
3 实验部分 8
3.1 实验仪器与试剂 8
3.2 实验方案设计 8 二甲基二烯丙基氯化铵中烯丙基类杂质形成机理初探:http://www.751com.cn/huaxue/lunwen_22183.html