2，2—二羥甲基丁酸的制備研究.pdf

1、天津大學碩士學位論文2，2—二羥甲基丁酸的制備研究姓名：陳二霞申請學位級別：碩士專業(yè)：化學工程指導(dǎo)教師：宋寶東20090601ABSTRACT2，2一Dimethylolbutanoicacid(DMBA)，alsoknownas22Bis(hydroxymethyl)butyricacidwhichhaslowmeltingpointandgooddissolubilityAsanewfinechemicalintermediate，

2、Itwouldtaketheplaceof22一dimethylolpropionicacidinpreparationofwaterbornepolyurethane，watersolublepolyesteradhesiveandcoatingagentandsoon2，2一dihydroxymethylbutanal(DMB)waspreparedbyaldolcondensationwithformaldehyde(FA)and

3、butyraldehyde(BA)undertheactionofalkalinecatalystsGaschromatography(CJC)methodWasestablishedandappliedtOmonitorthechemicalcompositionsofthereactionmixtureIthasbeenfoundthat：(1)weobtainedtheoptimumconditionsofaldolcondens

4、ationthroughorthogonalexperimentwhenusedtrimethylamineascatalystwhichincludedthatthemolarratioofFAtoBAandTMAtoBAwere25：1andO1：1respectivelythetemperatureWaS40“Candreactedfor45h，andthemolaryieldofDMBreached613％(2)ithadabe

5、ttermolaryieldwhenusedanion—exchangeresinD311ascatalystThebesttechnologyconditionswerethat：themolarratioofFAtoBAWaS4：1，theoptimalsolventwatertoBAmolarratiowas12：1，themolaryieldofDMBwasupto769％onthebasisofBA，whenthereacti

6、onWasconductedat50℃for5hDMBAwassynthesizedbyoxidationofDMBwithhydrogendioxide，thenwefinallygotwhitecrystalthroughvacuumdistillation，crystallizationandre—crystallizationIthasbeenfoundthat血ebestmolarratioofH202toDMBwas12：1

7、，theoptimalvolumeratioofwatersolventtODMBwas1：1ThemolaryieldofDMBAWaSupto696％whentheoxidationreactionWasconductedat70℃for6hundertheoptimalconditionsThestructureofDMBAwascharacterizedbyIRandNMRandHighPerformanceLiquidChro

8、matography(HPLC)wasusedforanalyzingthecontentofDMBAinordertocalculateitsmolaryieldSomepropertiesoftheproduct，includinghydroxylvalue，aciditymeltingpointandashcontentwhichweremeasuredusingchemicalanalysisapproachesTheresul