聚苯乙烯-二乙烯苯接枝聚乙二醇催化合成对硝基苯甲醚

Synthesis of Polystyrene-supported Polyethylene Glycol and its Application in Synthesis of p-Nitroanisole

探素了诸因素对制备催化剂过程的影响，合成出了聚苯乙烯－二乙烯苯接枝PEG－400并以此为三相转移催化剂。研究了对硝基苯甲醚的合成工艺，考察了催化剂，氢氧化钠、甲醇用量等对反应转化率的影响，建立了较佳合成工艺条件，即:n(PNCB):n(CH3OH):n(NaOH):n(PEG-400)=1:3:3:0.03-0.05,反应温度－80℃，反应时间9－10h。该条件下，对硝基氯苯转化率＞99．5％，以对硝基氯苯计，对硝基苯甲醚收率＞95％，气相色谱分析产品纯度99．7％。聚苯乙烯－二乙烯苯接枝PEG－400催化剂可重复使用5次以上，母液除盐后用于配碱对反应无不良影响。

Polystyrene-supported polyethylene glycol-400 (PEG-400) used as tri-phase transfer catalyst (TPTC) was synthesized. Effects of many factors on synthesis process of polystyrene-supported PEG-400 was also discussed. In the presence of sodium hydroxide, synthesis process of p-nitroanisole by reaction of p-nitrochlorobenzene(PNCB) and methanol, using polystyrene-supported PEG-400 as TPTC, was investigated. Effects of amounts of catalyst, sodium hydroxide and methanol etc. on reaction conversion rate was also studied. The optimum reaction condition was obtained, that is: n(PNCB): n(CH3OH): n(NaOH): n(PEG-400)=1:3:3: (0.03~0.05), reaction temperature is about 80℃, time 9~10h. The yield of p-nitroanisole calculated by amounts of p-nitrochlorobenzene is over 95% and the purity of p-nitroanisole is about 99.7% by GC analysis. The polystyrene-supported polyethylene glycol-400 catalyst may be used more than 5 times. After desalting, water fluid remained in the reactor can be used to make up sodium hydroxide solution and can be continuously reused in the above-motioned synthesis process.