磺酸型树脂固定床连续催化二壬基酚烷基转移反应的研究
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摘要
以壬基酚装置精馏塔釜底液为原料,以磺酸型聚苯乙烯阳离子交换树脂为催化剂,采用常压固定床连续工艺,开展二壬基酚与苯酚的烷基转移反应研究制取壬基酚。分别采用红外光谱、差热热重分析、催化剂颗粒强度测试等表征方法对催化剂的组成、热稳定性及力学性能进行研究。考察了反应温度、原料配比、质量空速和反应时间等因素对催化性能的影响。结果表明,所制备的树脂具有良好的热稳定性和耐压强度,适用于180℃以下的固定床连续反应工艺。在反应温度为160℃、原料质量空速为1h~(-1)、苯酚与二壬基酚质量比为3:1的条件下,二壬基酚转化率达85.9%~90.6%,壬基酚收率达56.8%~67.2%,催化剂稳定性好,连续反应200h催化性能仍保持稳定。
The transalkylation of dinonylphenol with phenol was carried out using a continuous fixed bed reactor, catalyzed by sulfonie acid ion exchange polystyrene resin. The composition,thermal properties and mechanical properties of sulfonated resin were characterized by FT-IR,TG-DTA and particle strength test. Effects of reaction temperature, raw materials ratio, space velocity and reaction time on the catalytic performance were investigated. The results show that prepared sulfonie acid ion exchange resin has excellent heat resistance and compressive strength,which is suitable for a continuous fixed bed reaction below 180℃. Under optimum conditions(reaction temperature 160℃, space velocity 1 h~(-1), and the phenol to dinonylphenol ratio 3), the conversion of dinonylphenol was up to 85.9%~90.6%, and the yield of nonylphenol was56.8%~67.2%. The resin catalyst shows excellent catalytic stability after 200 h continuous experiment.
The transalkylation of dinonylphenol with phenol was carried out using a continuous fixed bed reactor, catalyzed by sulfonie acid ion exchange polystyrene resin. The composition,thermal properties and mechanical properties of sulfonated resin were characterized by FT-IR,TG-DTA and particle strength test. Effects of reaction temperature, raw materials ratio, space velocity and reaction time on the catalytic performance were investigated. The results show that prepared sulfonie acid ion exchange resin has excellent heat resistance and compressive strength,which is suitable for a continuous fixed bed reaction below 180℃. Under optimum conditions(reaction temperature 160℃, space velocity 1 h~(-1), and the phenol to dinonylphenol ratio 3), the conversion of dinonylphenol was up to 85.9%~90.6%, and the yield of nonylphenol was56.8%~67.2%. The resin catalyst shows excellent catalytic stability after 200 h continuous experiment.
引文
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[2]尹芳华,陈群,杨扬,等.合成壬基酚的新催化工艺研究.石油化工[J].1998,27(10):707-709.
[3]王红秋.壬基酚的生产与应用.广州化工[J].2001,29(1):37-38.
[4]黄振军,王贵军.国内壬基酚的生产技术及新进展.精细石油化工进展[J].2001,2(4):46-49.
[5]陈淑芬.壬基酚的生产工艺及应用现状.兰州石化职业技术学院学报[J].2000,(1):15-19.
[6]崔文峰.二壬基酚聚氧乙烯醚的合成与应用.石油化工[J].1996,25(10):723-727.
[7]Guy D B,Renan B B.Lubricating composition,preparation process and applications,particularly as an additive in oils[P].US 5484544,1996.
[8]Salvatore A.Hydrocarbon fuel additive[P].US 4808195,1989.
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[10]刘岭梅.壬基酚市场应用及生产技术概述.浙江化工[J].2003,34(3):24-26.
[11]龚云表,石安富编著.合成树脂与塑料手册[M].上海:上海科学技术出版社,1993.
[12]徐斌,刘艳秋,王俊格,等.胺化改性磺酸型阳离子交换树脂酸碱协同催化环己酮自缩合反应.高校化学工程学报[J].2015,29(2):335-340.
[13]Joseph F M K,Petrus A M J S,Jozef A T.Process for preparing2-(1-cyclohexenyl)-cyclohexanone[P].US 4052458,1976.
[14]王浩亮.磺酸型聚苯乙烯阳离子交换树脂连续催化3-甲基-1-戊烯-4-炔-3-醇转位重排反应研究.化学工程与装备[J].2017,(6):25-28.
[15]何明阳,陈群,杨绪杰,等.耐温阳离子树脂催化二壬基酚与苯酚合成壬基酚.离子交换与吸附[J].2003,19(5):444-449.