三(羟甲基)硝基甲烷的合成工艺研究摘要：到目前为止，国内外生产三(羟甲基)硝基甲烷(TN)的工艺条件还不够好，存在杂质多、生产时间长、产量低、副反应、质量不稳定等问题。本文对三(羟甲基)硝基甲烷(TN)的生产工艺条件进行优化，使用甲醛溶液滴入到硝基甲烷溶液中的方法，把氢氧化钙做为催化剂。综合考察了亲核加成反应的反应时间、物料比、反应温度、催化剂、pH值等五个因素对产率的影响。得到最新的工艺条件：反应原料滴加顺序为甲醛滴入硝基甲烷中，甲醛溶液与硝基甲烷溶液物质的量之比为3.2：1、溶剂为水、反应时间5小时、反应催化剂为氢氧化钙、反应温度40℃、用硫酸除去钙离子、产率高达89.1%。关键词：三(羟甲基)硝基甲烷；合成；工艺条件；亲核加成StudyonsynthesistechnologyoftrimethylolnitromethaneAbstract:Uptonow,theprocessconditionsfortheproductionoftrimethylolnitromethane(TN)athomeandabroadarenotgoodenough.Therearemanyproblemssuchasmanyimpurities,longproductiontime,lowyield,sidereactionsandunstablequality.Inthispaper,theproductionconditionsoftrimethylolnitromethane(TN)wereoptimized.Themethodofdroppingformaldehydesolutionintonitromethanesolutionwasused.Calciumhydroxidewasusedasthecatalyst.Theeffectsofreactiontime,materialratio,reactiontemperature,catalystandpHvalueonyieldwereinvestigated.Getthenewesttechnologicalconditions:reactionrawmaterialaddorderforformaldehydedropsintothenitromethane,molarratioofformaldehydesolutionandnitromethanesolutionratioof3.2:1,thesolventiswater,thereactiontime5hours,reactionofcalciumhydroxidecatalyst,reactiontemperature40℃,withsulfuricacidtoremovecalciumandproductionrateashighas89.1%.Keywords:Trimethylolnitromethane;Synthesis;Processconditions;Nucleophilicaddition目录1引言.................................................................................................................11.1三(羟甲基)硝基甲烷的结构及性质...........................................................11.2三(羟甲基)硝基甲烷的用途.......................................................................11.3三(羟甲基)硝基甲烷的合成方法...............................................................21.4三羟甲基硝基甲烷合成的基本原料.........................................................21.5国内研究概况.............................................................................................31.6研究内容及意义.........................................................................................52实验部分........................................................................................................62.1实验仪器与药品.........................................................................................62.1.1实验仪器..................................................................................................62.1.2实验药品..................................................................................................62.2三(羟甲基)硝基甲烷的合成.......................................................................73结果与讨论....................................................................................................83.1三(羟甲基)硝基甲烷产率的影响因素.......................................................83.1.1反应物添加方式对三(羟甲基)硝基甲烷产率的影响............................83.1.2甲醛与硝基甲烷的物质的量的比对反应产率的影响..........................83.1.3催化剂的不同对三(羟甲基)硝基甲烷产率的影响................................93.1.4不同的反应时间对三(羟甲基)硝基甲烷产率的影响..........
