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新型沥青乳化剂和沥青抗剥落剂的合成与性能表征
Synthesis and Performance Characterization of Novel Asphalt Emulsifiers and Anti-stripping Agent
【作者】 怀春雷;
【导师】 施来顺;
【作者基本信息】 山东大学 , 化学工艺, 2013, 硕士
【摘要】 本文合成了一种甜菜碱型两性沥青乳化剂、一种阳离子型沥青乳化剂和一种磷酸酯类沥青抗剥落剂。探究了各反应参数对反应收率的影响,得出了最佳合成路线。利用在线红外对反应进行跟踪检测,对反应过程进行了理论分析。利用静态红外光谱对各反应产物进行了结构鉴定。利用表面张力法测定了产品乳液的临界胶束浓度(CMC),对乳化剂的乳化性能进行了检测,利用水煮法对抗剥落剂的抗剥落性能进行了测试。以月桂醇、环氧氯丙烷、二甲胺、氯乙酸经三步反应合成出一种新型甜菜碱型沥青乳化剂3-(十二烷氧基)-2-羟基丙基-N-乙酸基-N,N-二甲基氯化铵。探究了各反应参数对第一步合成2-(十二烷氧基亚甲基)环氧乙烷的收率影响,确定了最佳合成路线。利用红外光谱对三种产物结构进行了表征,利用在线红外光谱技术对第一步合成2-(十二烷氧基亚甲基)环氧乙烷的反应进行了追踪分析。测定了产品乳液的临界胶束浓度(CMC)和该浓度下的表面张力大小。乳化性能检测结果显示,该乳化剂对沥青具有很好的乳化能力,制备的乳化沥青储存稳定性良好,属于中裂型沥青乳化剂。以十八烷基二甲基叔胺、环氧氯丙烷、二甲胺水溶液经两步反应合成出一种新型阳离子沥青乳化剂N-(3-(N’,N’-二甲基氨基)-2-羟基丙基)-N,N-二甲基十八烷基-1-氯化铵。利用红外光谱对两种产物结构进行了表征,利用在线红外技术对第一步合成N,N-二甲基-N-(环氧乙烷-2-亚甲基)十八烷基-1-氯化铵的反应进行了追踪分析。测定了产品乳液的临界胶束浓度(CMC)和该浓度下的表面张力大小。乳化沥青电荷测试表明,该乳化产品带有正电荷。乳化性能检测结果显示,该乳化剂对沥青具有很好的乳化能力,制备的乳化沥青储存稳定性良好,属于中裂型沥青乳化剂。以五氧化二磷和月桂醇为原料经酯化反应合成十二烷基磷酸酯混合物,对磷酸酯混合物中的十二烷基焦磷酸酯进行水解反应,得到以单十二烷基磷酸酯为主要活性成分的沥青抗剥落剂。以单十二烷基磷酸酯为目标产物,探究了各反应参数对产物收率的影响,确定了最佳合成路线。利用红外光谱对单十二烷基磷酸酯结构进行了表征;利用在线红外光谱技术对酯化反应和水解反应进行了跟踪分析。水煮法抗剥落性能测试表明,该磷酸酯类沥青抗剥落剂具有较好的抗剥落能力。
【Abstract】 A novel betaine-type asphalt emulsifier, a cationic asphalt emulsifier and a asphalt anti-stripping agent were synthesized in this paper. The optimum reaction conditions were obtained by the close investigation of various factors that influenced the reaction yield. The reactions were tested by React IR to get theoretical data. The structures of the products were identified by FTIR. The performance tests of emulsifiers and anti-stripping agent were investigated in the mixing test with rock material.A novel betaine-type asphalt emulsifier,3-(dodecyloxy)-2-hydroxypropan-N-carboxymethyl-N,N-dimethylammonium chloride, was synthesized in a three-step reaction from lauryl alcohol, epichlorohydrin, dimethylamine, and chloroacetic acid. The optimum reaction conditions were obtained for synthesis of2-(dodecyloxymethyl)-oxirane in the first step. The structures of the three products were identified by FTIR. Synthesis of2-(dodecyloxymethyl) oxirane in the first step was monitored by online FTIR, and an intermediate was detected. The CMC of the emulsifier and the surface tension at CMC were determined by the surface tension method. The performance research indicated the product is an excellent emulsifier for asphalt. The prepared bituminous emulsion had high storage stability. The emulsifier is a medium-set asphalt emulsifier.A novel cationic asphalt emulsifier N-(3-(N’,N’-dimethylamino)-2-hydroxypropyl)-N,N-dimethyloctadecan-l-aminium chloride was synthesized in a two-step reaction of epichlorohydrin, N,N-dimethyloctadecylamine, and dimethylamine aqueous solution. The structures of the products were identified by FTIR. The first synthesis step of N,N-dimethyl-N-(oxiran-2-ylmethyl)octadecan-l-aminium chloride was monitored by online FTIR. The CMC of the emulsifier and the surface tension at CMC were determined by the surface tension method. The performance research indicated the product an excellent emulsifier for asphalt. The prepared bituminous emulsion had high storage stability. The emulsifier belongs to medium-set asphalt emulsifier.A novel phosphate type asphalt anti-stripping agent was synthesized in a two-step reaction from phosphorus pentaoxide and lauryl alcohol. Mixed phosphates were synthesized in the first step and the pyrophosphates were hydrolyzed in the second step. The optimum reaction conditions were obtained for synthesis of phosphate monoester. The structure of the phosphate monoester was identified by FTIR. The reactions were monitored by online FTIR. The performance research indicated the anti-stripping agent had strong anti-stripping power.
【Key words】 Asphalt; Emulsifier; Anti-stripping Agent; Synthesis; Online FTIR;