本文選題：瀝青 + 乳化劑��； 參考：《山東大學(xué)》2015年碩士論文

【摘要】：本文合成了四種新型陽離子瀝青乳化劑。研究了影響反應(yīng)產(chǎn)率的因素,并得到了最佳的反應(yīng)條件。利用紅外光譜、1H NMR,元素分析對產(chǎn)物結(jié)構(gòu)進行了表征,利用在線紅外光譜技術(shù)對反應(yīng)進行追蹤檢測,提出了合理的反應(yīng)機理。利用表面張力法和電導(dǎo)法分別測定了產(chǎn)物的表面張力和電導(dǎo)率,得出了產(chǎn)物的臨界膠束濃度(CMC),并對乳化劑的乳化性能進行了測試。以壬基酚聚氧乙烯醚(NP-10)、壞氧氯丙烷和三乙胺反應(yīng)合成出一種新型陽離子瀝青乳化劑N-(、3-壬基酚聚氧乙烯醚(10)-2-羥基)丙基-N,N,N-三乙基氯化銨。確定了最佳反應(yīng)條件為：反應(yīng)時間8 h,反應(yīng)溫度70℃,氫氧化鈉與NP-10的摩爾比1.0,環(huán)氧氯丙烷與NP-10的摩爾比1.2,三乙胺與NP-10的摩爾比1.2。在最佳工藝條件下產(chǎn)率可達(dá)48.72%。利用紅外光譜對產(chǎn)物結(jié)構(gòu)進行了表征。利用在線紅外光譜技術(shù)對合成反應(yīng)進行跟蹤分析,檢測出中間體�；谝陨蠈嶒灁�(shù)據(jù),提出了合理的反應(yīng)機理。產(chǎn)物N-(3-壬基酚聚氧乙烯醚(10)-2-羥基)丙基-N,N,N-三乙基氯化銨的臨界膠束濃度通過表面張力法測定,產(chǎn)物的臨界膠束濃度(CMC)為1.19×10-3 mol/L,其數(shù)值較小,在臨界膠束濃度下表面張力為40.13 mN/m。對該乳化劑進行了乳化性能測試。性能測試表明：這種乳化劑對瀝青具有很好的乳化能力,制備的乳化瀝青具有良好的儲存穩(wěn)定性,可拌和時間大于2 min,屬于慢裂型瀝青乳化劑。以十八胺、丙烯酸、氯乙酸為原料通過兩步反應(yīng)合成出一種新型瀝青乳化劑十八烷基-雙(2-羧乙基)-羧甲基氯化銨。確定了合成第一步產(chǎn)物十八烷基二丙酸基叔胺的最佳反應(yīng)條件為：反應(yīng)溫度70℃,反應(yīng)時間5 h,丙烯酸與十八胺的摩爾比2.2。在最佳反應(yīng)條件下,產(chǎn)率可達(dá)52.39%。利用FTIR/1HNMR和元素分析對產(chǎn)物結(jié)構(gòu)進行了表征。利用在線紅外光譜技術(shù)對合成第一步產(chǎn)物十八烷基二丙酸基叔胺的反應(yīng)進行了跟蹤分析,檢測出中間產(chǎn)物。基于以上實驗數(shù)據(jù),提出了合理的反應(yīng)機理。利用電導(dǎo)法測得產(chǎn)物十八烷基-雙(2-羧乙基)-羧甲基氯化銨的臨界膠束濃度為2×10-3 mol/L,其值較小。對該乳化劑進行了乳化性能測試。性能測試表明：十八烷基-雙(2-羧乙基)-羧甲基氯化銨與NP-10按一定比例復(fù)配,該復(fù)配后的乳化劑對AH-90瀝青具有很好的乳化能力,制備的乳化瀝青具有很好的貯存穩(wěn)定性。拌和時間為15 s,表明該乳化劑是一種快裂型瀝青乳化劑。以十八胺、環(huán)氧丙烷、氯乙酸鈉為原料通過兩步反應(yīng)合成出一種新型瀝青乳化劑十八烷基-雙(2-羥基丙基)-乙酸鈉基氯化銨。確定了合成十八烷基-雙(2-羥基丙基1-乙酸鈉基氯化銨第二步的最佳反應(yīng)條件為：反應(yīng)溫度75。C,反應(yīng)時間4 h,氯乙酸鈉與十八胺的摩爾1.1。在最佳反應(yīng)條件下,產(chǎn)率可達(dá)79.00%。利用FTIR、 1HNMR和元素分析對產(chǎn)物結(jié)構(gòu)進行了表征。利用在線紅外光譜技術(shù)對合成第一步產(chǎn)物十八烷基二丙酸基叔胺和第二步產(chǎn)物十八烷基-雙(2-羥基丙基)-乙酸鈉基氯化銨的反應(yīng)分別進行了跟蹤分析,檢測出中間產(chǎn)物。利用電導(dǎo)法測得產(chǎn)物十八烷基-雙(2-羥基丙基)-乙酸鈉基氯化銨的臨界膠束濃度為3.49×10-3 mol/L,其值較小。對該乳化劑進行了乳化性能測試。性能測試表明：該乳化劑對AH-90瀝青具有很好的乳化能力,制備的乳化瀝青具有很好的貯存穩(wěn)定性。拌和時間為15 s,表明該乳化劑是一種快裂型瀝青乳化劑。以壬基酚、三乙烯四胺、甲醛經(jīng)一步反應(yīng)合成出一種新型陽離子瀝青乳化劑2-三乙烯四胺基亞甲基-4-壬基苯酚。確定最佳合成條件為：反應(yīng)時間5 h,反應(yīng)溫度95℃,甲醛與壬基酚的摩爾比2.8,三乙烯四胺與壬基酚的摩爾比1.0。在最佳工藝條件下反應(yīng)的產(chǎn)率可達(dá)49.21%。利用紅外光譜對產(chǎn)物結(jié)構(gòu)進行了表征。對該乳化劑進行了乳化性能測試。性能測試表明：該乳化劑對AH-90瀝青具有很好的乳化能力,制備的乳化瀝青儲存穩(wěn)定性良好,拌和時間為90 s,屬于中裂型瀝青乳化劑。
[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.

【學(xué)位授予單位】：山東大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：U414

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