新型两性表面活性剂二烷基胺聚氧乙烯醚磷酸单醋钾盐的合成和性能测试.docx
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新型两性表面活性剂二烷基胺聚氧乙烯醚磷酸单醋钾盐的合成和性能测试
新型两性表面活性剂二烷基胺聚氧乙烯醚磷酸单醋钾盐的合成和性能测试
摘要
合成了两种国内文献未见报道的新型磷酸酷两性表面活性剂，并对其表面
活性及应用性能进行了测试。
在测试其表面活性及应用性能的基础上，对配方应
用实验进行了研究，得到了稳定的乳化膏霜，乳化松香和抗静电良好的纺丝油剂。
在合成方面，首先以N,N一二轻乙基十二胺为原料，通过三因素、三水平
的正交设计，选择出合成磷酸单一2-（N-轻乙基一N一十二烷基）氨基乙醋的
最佳实验条件，即以环己烷为溶剂，以聚磷酸为磷酸化剂，氮与磷的摩尔比为
1.2:
1，反应温度为1200C，反应时间为6小时，将磷酸单醋与氢氧化钾进行中
和反应，得到磷酸单醋钾盐，简称化合物（I）。
在此基础上，又以十二烷基胺聚
氧乙烯醚为原料合成了十二烷彝氧乙烯磷酸单酉旨钾盐，简称化合物（II）。
在
取得化合物（I）的最佳实验条件之后，对溶剂进行了筛选。
在合成化合物（（II）
时对磷酸化剂及氮与磷的摩尔比进行了探索。
在性能测试方面，主要测定了化合物（I）和化合物（（II）的表面张力和临
界胶束浓度（CMC）、润湿力、乳化力、抗静电性、去污力等，同时测定了化合
物（I）的等电点（（PD.测定结果表明化合物（I）具有良好的表面活性，同时具
有两性物质所共同具有的等电点的特征。
在偏酸性时，显现阳离子表面活性剂的
特征;在偏碱时，显现阴离子表面活性剂的特征;无论在酸性还是在碱性条件下，
均有很好的乳化力。
针对它突出的乳化力进行了应用实验，主要用于乳化膏霜配
方，化纤油剂和松香乳化，都取得了良好的效果，作为两性乳化剂，它比其他离
子型乳化剂的配伍性更好，还会赋予配方其他优良性质，是一个有前途的乳化剂。
化合物（（II）与原料十二烷基胺聚氧乙烯醚的各项性能比较接近，而且原料的CMC
要小于化合物（（II）的CMC，所以在目前已测性质基础上合成化合物（II）的应
用意义不大。
关键词:
两性表面活性剂，磷酸单醋钾盐，聚磷酸，乳化力
—一一一一北峨彭化J共大.学二醉」=掌n1V文一一一一一一一
NEWAMPHOTERICSURFACTANT:
DODECYL
AMINEPOLYXYETHYLENEMONO-PHOSPHATE
POTASSIUM:
SYNTHESISANDCHARACTERIZATION
ABSTRACT
Thispaperrelatestosynthesisoftwonewstructureamphoteric
phosphatesurfactantswhichhavenotbeenreportedincivilandtheir
surfaceactivityandappliedcapabilitieshavebeencharacterized.Onthe
basisofcharacterization,itresearchessomeformulationsandgetsstable
emulsioncreamandemulsionresinaandspinfinisheswhichhaswell
antistaticability.
Theamphotericmono-2-（N-ethanol-N-dodecyl）aminoethyl
phosphatehasbeenpreparedbyreactingN-dodecyl-N,N-diethanolamine
withpolyphosphoricacid.Throughorthogonaldesignwhichincludes
three睡AlvrSthreelevels,thepreferablereactionroutinehasbeen
achieved,whichcontainscyclohexaneassolvent,in-situpolyphosphoric
acidasphosphationreagent,molarratioofnitrogentophosphorusis
1.2:
1,tempratureis1200C，andthetimeis6hours.Thephosphatewillbe
neutralizedbypotassiumhydroxide，andtheproductwillbecalled
compound（I）.Thecompound（II）,namelydodecylamine
polyoxyethylenemono-phosphatepotassiumhasbeenpreparedby
乙
—一一一一斗匕一哀北-工大学迫瓦土Ift-1iA}E一一一一一一
phosphatingpolyoxyethylenedodecylamineandneutralizingwithbase.
Inordertoselecttheoptimumconditionofpreparationofcompound（I）,
differentsolventhasbeentestedaswellphosphationagentandmolar
ratio肠fnitrogentophosphorusduringpreparingthecompound（II）.
Aseriesofexperimentshavebeenmadetotestifythesesurfactants'
surfaceactivitiesandappliedcapabilitie斌Itcangive。
conclusionthat
compound（I）hasgoodbehaviorsuchashigherdetersivepower,
emulsifyingpowerandantistaticpower.Ithasisoelectricpoint（pI）which
ischaracterofamphotericsubstances.WhilethepHofsolutionismore
thanseven,itshowsasanionicsurfactants;andwhilethepHofsolution
islessthanseven,itshowsascationicsurfactant.Whateverthesolutionis
acidicorbasic,thecompound（I）alwaysshowsverygoodemulsifying
power.Inthelightofcompound
（1）'spreferableemulsifyingpower,the
formulationhavebeenmademainlyinemulsioncreamandemulsion
resinaandspinfinisheswhichhaveachievegoodresults.Asan
amphotericsurfactantithasbettercooperativeeffectsthanotherionic
surfactantsandalsogivestheformulationsgoodcharacter,whichhas
testifiedthecompound（I）isacompromisingsurfactant.Comparingthe
compound（II）withitsrawmaterial,itcanbeenfoundthatcompound（II）
hasthesimilarsurfaceactivityandappliedcapabilities.Itsrawmaterial's
criticalmicelleconcentrationissmallerthanits.Italsocangivea
conclusionthatthepreparationofcompound（II）isimpractical.
-一一一一一华眼京习犯T,大渭爵
KEYWORDS:
amphotericsurfactant,mono-phosphatepatassium,
polyphosphoricacid,emulsifyingpower
北京化工大学硕士学位论文
目录
第一章前言·................................................................................
（1）
1.1表面活性剂概述·································································……
（1）
1.1.1表面活性剂的结构特点及其性能··········································……
（1）
1.1.2表面活性剂的分类···……”·················································……
（1）
1.1.3两性表面活性剂的特点······················································……（3）
1.2磷酸酷表面活性剂·······························································……（4）
1.2.1磷酸酷类表面活性剂的结构特点及分类·································……（4）
1.2.2磷酸酷类表面活性剂的合成路线··········································……（5）
1.2.3磷酸酷盐的用途·······························································……（8）
1.3论文选题的目的和意义·..............................................................（9）
第二章实验部分·..........................................................................（11）
2.1磷酸酷盐两性表面活性剂的合成··········································……（11）
2.1.1实验仪器和药品············。
···············································……c11）
2.1.2实验方法·····································································……（11）
2.2磷酸酷含量的测定····························································……（13）
2.2.1原理···········································································……（13）
2.2.2仪器··················。
························································……（14）
2.2.3药品···········································································……（14）
2.2.4实验方法·····································································……（15）
2.3产物的表面性质测定·························································……（15）
2.3.1表面张力的测定····························································……（15）
2.3.2润湿能力的测定······························，·····························……（17）
2.3.3等电点的测定·······························································……（19）
2.4产物应用性能的测定·························································……（21）
2.4.1乳化力的测定·······························································，··…X21）
2.4.2抗静电性测定·······························································……（22）
2.4.3去污力的测定·····，·························································……（2:
3）
第1页
北京化工大学硕士学位论文
2.4.4泡沫力的测定（ROSS-MILES法）.······································……（25）
2.5应用配方实验··································································……（28）
2.5.1乳化膏霜的制备及稳定性测试··········································……（28）
2.5.2纺丝油剂的配方实验······················································……（28）
2.5.3松香乳化实验·······························································……（29）
2.6结构测定········································································……（31）
2.6.1红外吸收光谱测定·························································……（31）
2.6.2核磁共振波谱测定·························································……（31）
第三章结果与讨论·.......................................................................（32）
3.1磷酸单一2-（N-轻乙基一N一十二烷基）
氨基乙酷的合成······························································……（32）
3.1.1磷酸单一2-（N-经乙基一N一十二烷基〕
氨基乙醋的合成条件的选择················································……（32）
3.1.2溶剂的筛选·················································。
················……（33）
3.1.3小结···········································································……（34）
3.2十二烷基胺聚氧乙烯醚磷酸单酷的合成·································……（34）
3.3产物物化性能的测定·························································……（35）
3.3.1表面张力的测定结果······················································……（35）
3.3.2润湿力的测定结果·························································……（38）
3.3.3等电点的测定结果·························································……（39）
3.4应用性能的测定结果·························································……（39）
3.4.1化合物（I）及化合物（I’）的应用
性能测试结果·......................................................................（40）
3.4.2不同反应溶剂对化合物（I）应用性能的影响·····················……（42）
3.4.3十二烷基胺聚氧乙烯醚磷酸单醋钾盐
的应用性能的测定·................................................................（43）
3.4.4不InI磷酸化试剂对反应的影响··········································……（44）
3.4.5小结··························，················································……（44）
3.5应用配方实验···················································。
··············……（40）
第2页
北京化工大学硕士学位论文
3.5.1乳化膏霜配方及稳定性比较·············································……（45）
3.5.2纺丝油剂的配方及测定结果·············································……（46）
3.5.3松香乳化实验的结果······················································……（47）
3.6分子结构的测定结果·..............................................................（47）
3.6.1红外吸收光谱测定结果···················································……（48）
3.6.2核磁共振波谱测定结果······························.·····················……（49）
3.6.3小结···········································································……（50）
第四章结论·.............................................................................（51）
参考文献····························································。
·················……（52）
致谢····················································································……（56）
就读硕士研究生期间发表的学术论文··········································……（57）
第3页
北京化工大学硕士学位论文
第一章前言
磷酸酷类阴离子表面活性剂，由于具有很高的表面活性、抗静电性和防锈
性，己被广泛应用于各工业领域〔‘一。
常见的品种有烷基磷酸醋盐和脂肪醇醚磷
酸酷盐等，如PK,NEP-7等。
近年来，国外对以磷酸醋盐为阴离子的两性表
面活性剂进行了较为广泛的开发和研究[3-4），认为这类表面活性剂从皮肤溶出的
氨基酸量少，脱脂低，毒性和刺激性特别低，而且表面活性如乳化、抗静电、润
湿性能良好，可以用于化妆品，洗涤用品以及纺织工业等诸多方面，因此越来越
受到人们的重视。
磷酸酷两性表面活性剂，无论在合成或是在性能、应用方面，
在国内工作开展甚少[5]，仅处于起步阶段，所以对磷酸酷类两性表面活性剂的研
究是很有必要的。
表面活性剂概述
1.1.1表面活性剂的结构特点及其性能[[6]
表面活性剂是指那些在较低浓度时就能使体系的表面张力明显降低的物
质。
它在结构上的特点是同时具有亲水性的极性基团和疏水性（或者说亲油性）
的非极性基团，所以表面活性剂是具有两亲结构的分子。
正是由于这种结构上的
两亲特性，使表面活性剂具有以下两种基本性质:
（1）它能在界面发生吸附，基
于官能团的定向选择吸附，使界面的状态或性质发生显著变化;
（2）当其浓度达
到一定范围时，即形成胶束。
表面活性剂所具有的润湿、乳化、起泡、消泡、分
散悬浮、凝聚以及洗涤等诸多实用性能，都与表面活性剂的这一两亲结构的特性
有关。
1.1.2表面活性剂的分类川
表面活性剂有多种分类方法，分类依据多种多样，但通常以亲水基团的结构
作为分类依据。
按亲水基是否带电将表面活性剂分为离子型和非离子型两大类。
第t页
北京化工大学硕士学位论文
离子型表面活性剂在水中能电离出带电的活性基团。
非离子表面活性剂在水中不
电离，呈电中性。
根据离子型表面活性剂在水中所带电荷的正负性，又可以将其
分成阴离子表面活性剂、阳离子和两性表面活性剂。
下表概略给出表面活性剂的
分类及举例。
表1一1表面活性剂的分类及举例
R-COONa
梭酸盐
R一S03Na
磺酸盐
阴离子表面活性剂
R一OS03Na
硫酸盐
R-OP03Na2
磷酸盐
+
R-NH2HCl
伯胺盐
+
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