新型阳离子沥青乳化剂的合成与研究

发布时间：2018-04-26 18:14

本文选题：沥青 + 乳化剂　；参考：《山东大学》2015年硕士论文

【摘要】：本文合成了四种新型阳离子沥青乳化剂。研究了影响反应产率的因素,并得到了最佳的反应条件。利用红外光谱、1H NMR,元素分析对产物结构进行了表征,利用在线红外光谱技术对反应进行追踪检测,提出了合理的反应机理。利用表面张力法和电导法分别测定了产物的表面张力和电导率,得出了产物的临界胶束浓度(CMC),并对乳化剂的乳化性能进行了测试。以壬基酚聚氧乙烯醚(NP-10)、坏氧氯丙烷和三乙胺反应合成出一种新型阳离子沥青乳化剂N-(、3-壬基酚聚氧乙烯醚(10)-2-羟基)丙基-N,N,N-三乙基氯化铵。确定了最佳反应条件为：反应时间8 h,反应温度70℃,氢氧化钠与NP-10的摩尔比1.0,环氧氯丙烷与NP-10的摩尔比1.2,三乙胺与NP-10的摩尔比1.2。在最佳工艺条件下产率可达48.72%。利用红外光谱对产物结构进行了表征。利用在线红外光谱技术对合成反应进行跟踪分析,检测出中间体。基于以上实验数据,提出了合理的反应机理。产物N-(3-壬基酚聚氧乙烯醚(10)-2-羟基)丙基-N,N,N-三乙基氯化铵的临界胶束浓度通过表面张力法测定,产物的临界胶束浓度(CMC)为1.19×10-3 mol/L,其数值较小,在临界胶束浓度下表面张力为40.13 mN/m。对该乳化剂进行了乳化性能测试。性能测试表明：这种乳化剂对沥青具有很好的乳化能力,制备的乳化沥青具有良好的储存稳定性,可拌和时间大于2 min,属于慢裂型沥青乳化剂。以十八胺、丙烯酸、氯乙酸为原料通过两步反应合成出一种新型沥青乳化剂十八烷基-双(2-羧乙基)-羧甲基氯化铵。确定了合成第一步产物十八烷基二丙酸基叔胺的最佳反应条件为：反应温度70℃,反应时间5 h,丙烯酸与十八胺的摩尔比2.2。在最佳反应条件下,产率可达52.39%。利用FTIR/1HNMR和元素分析对产物结构进行了表征。利用在线红外光谱技术对合成第一步产物十八烷基二丙酸基叔胺的反应进行了跟踪分析,检测出中间产物。基于以上实验数据,提出了合理的反应机理。利用电导法测得产物十八烷基-双(2-羧乙基)-羧甲基氯化铵的临界胶束浓度为2×10-3 mol/L,其值较小。对该乳化剂进行了乳化性能测试。性能测试表明：十八烷基-双(2-羧乙基)-羧甲基氯化铵与NP-10按一定比例复配,该复配后的乳化剂对AH-90沥青具有很好的乳化能力,制备的乳化沥青具有很好的贮存稳定性。拌和时间为15 s,表明该乳化剂是一种快裂型沥青乳化剂。以十八胺、环氧丙烷、氯乙酸钠为原料通过两步反应合成出一种新型沥青乳化剂十八烷基-双(2-羟基丙基)-乙酸钠基氯化铵。确定了合成十八烷基-双(2-羟基丙基1-乙酸钠基氯化铵第二步的最佳反应条件为：反应温度75。C,反应时间4 h,氯乙酸钠与十八胺的摩尔1.1。在最佳反应条件下,产率可达79.00%。利用FTIR、 1HNMR和元素分析对产物结构进行了表征。利用在线红外光谱技术对合成第一步产物十八烷基二丙酸基叔胺和第二步产物十八烷基-双(2-羟基丙基)-乙酸钠基氯化铵的反应分别进行了跟踪分析,检测出中间产物。利用电导法测得产物十八烷基-双(2-羟基丙基)-乙酸钠基氯化铵的临界胶束浓度为3.49×10-3 mol/L,其值较小。对该乳化剂进行了乳化性能测试。性能测试表明：该乳化剂对AH-90沥青具有很好的乳化能力,制备的乳化沥青具有很好的贮存稳定性。拌和时间为15 s,表明该乳化剂是一种快裂型沥青乳化剂。以壬基酚、三乙烯四胺、甲醛经一步反应合成出一种新型阳离子沥青乳化剂2-三乙烯四胺基亚甲基-4-壬基苯酚。确定最佳合成条件为：反应时间5 h,反应温度95℃,甲醛与壬基酚的摩尔比2.8,三乙烯四胺与壬基酚的摩尔比1.0。在最佳工艺条件下反应的产率可达49.21%。利用红外光谱对产物结构进行了表征。对该乳化剂进行了乳化性能测试。性能测试表明：该乳化剂对AH-90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,拌和时间为90 s,属于中裂型沥青乳化剂。
[Abstract]:Four new cationic asphalt emulsifiers were synthesized. The factors affecting the yield of the reaction were studied and the optimum reaction conditions were obtained. The structure of the products was characterized by infrared spectroscopy, 1H NMR, element analysis, and the reaction was traced by the on-line infrared spectroscopy. The rational reaction mechanism was put forward and the surface tension was used. The surface tension and conductivity of the products were measured by method and conductivity method, and the critical micelle concentration (CMC) was obtained. The emulsifying properties of the emulsifier were tested. A new cationic asphalt emulsifier N- (3- nonylphenol polyoxyethylene ether (10) was synthesized by the reaction of nonylphenol polyoxyethylene ether (NP-10), oxychloropropane and three ethylamine. -2- hydroxy) propyl -N, N, N- three ethyl ammonium chloride. The optimum reaction conditions are as follows: reaction time 8 h, reaction temperature 70, molar ratio of sodium hydroxide to NP-10 1, molar ratio of epoxy chloropropane to NP-10 1.2, and the molar ratio 1.2. of three ethylamine and NP-10 in the optimum process conditions to 48.72%. using infrared spectra for product structure Based on the above experimental data, a reasonable reaction mechanism was proposed. The critical micelle concentration of the product N- (3- nonylphenol polyoxyethylene ether (10) -2- hydroxyl) propyl -N, N, N- three ethyl ammonium chloride was determined by surface tension method, and the critical micelle of the product The concentration (CMC) is 1.19 x 10-3 mol/L, and its value is smaller. The emulsifying property of the emulsifier is tested by the surface tension of 40.13 mN/m. under the critical micelle concentration. The performance test shows that the emulsifier has a good emulsifying ability to the asphalt, and the prepared emulsified asphalt has good storage stability, and the mixing time is more than 2 min, which belongs to the asphalt. Slow cracking asphalt emulsifier, a new asphalt emulsifier, eighteen alkyl - double (2- carboxyethyl) - carboxymethyl ammonium chloride, was synthesized from eighteen amine, acrylic acid and chloroacetic acid in two steps. The optimum reaction strip for the synthesis of the first step product, eighteen alkyl two propionate, was: reaction temperature 70, reaction time 5 h, acrylic acid With the molar ratio of eighteen amine to the molar ratio of 2.2., the yield can be up to 52.39%. by using FTIR/1HNMR and elemental analysis to characterize the structure of the product. The reaction of the first step product eighteen alkyl two propionate tertiary amine was tracked and the intermediate product was detected by the on-line infrared spectroscopy. Based on the above experimental data, A reasonable reaction mechanism was obtained. The critical micelle concentration of the eighteen alkyl - double (2- carboxyethyl) - carboxymethyl ammonium chloride was measured by the conductivity method of 2 x 10-3 mol/L, and its value was small. The emulsifying properties of the emulsifier were tested. The performance test showed that the eighteen alkyl - double (2- carboxyethyl) - carboxymethyl ammonium chloride was mixed with NP-10 in a certain proportion. The emulsifier after the compound has good emulsifying ability to AH-90 bitumen. The prepared emulsified asphalt has good storage stability. The mixing time is 15 s, indicating that the emulsifier is a fast cracking asphalt emulsifier. A new asphalt emulsifier eighteen alkane is synthesized by two steps with eighteen amine, epoxy propane and sodium chloroacetate as raw materials. Base double (2- hydroxypropyl) - sodium acetate ammonium chloride. The optimum reaction conditions for the synthesis of eighteen alkyl - double (2- hydroxypropyl 1- sodium acetate) ammonium chloride are the best reaction conditions: reaction temperature 75.C, reaction time 4 h, and molar 1.1. of sodium chloroacetate and eighteen amines at optimum reaction conditions, the yield can reach 79.00%. using FTIR, 1HNMR and elemental analysis The structure of the product was characterized. The reaction of the first step product eighteen alkyl two propionic acid base amine and the second step product eighteen alkyl - double (2- hydroxypropyl) - sodium ammonium acetate was followed by the on-line infrared spectroscopy, and the intermediate products were detected. The products of eighteen alkyl - double (2- hydroxyl group) were obtained by using the conductance method. The critical micelle concentration of propyl) sodium acetate is 3.49 x 10-3 mol/L, and its value is small. The emulsifying performance of the emulsifier is tested. The performance test shows that the emulsifier has a good emulsifying ability to AH-90 asphalt, and the emulsified asphalt prepared has a good storage stability. The mixing time is 15 s, indicating that the emulsifier is a one. A fast cracking asphalt emulsifier, with nonylphenol, three ethylene four amine, a new cationic asphalt emulsifier 2- three ethylene four amine methylene -4- nonyl phenol was synthesized by one step reaction. The optimum synthesis conditions were as follows: reaction time 5 h, reaction temperature 95, formaldehyde and nonylphenol molar ratio 2.8, three ethylene four amine and nonyl phenol. The yield of 1.0. is 49.21%. under the optimum conditions. The emulsifying property of the emulsifier is tested. The performance test shows that the emulsifier has a good emulsifying ability to AH-90 bitumen, the storage stability of the emulsified asphalt is good and the mixing time is 90 s. Medium split asphalt emulsifier.

【学位授予单位】：山东大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：U414

【相似文献】