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悬浮法合成苯并恶嗪中间体工程化研究
Chemical Engineering in Suspension Polymerization of Benzoxazine Intermediate
【作者】 王昌花;
【导师】 向福如;
【作者基本信息】 四川大学 , 化学工程, 2001, 硕士
【摘要】 由苯并恶嗪中间体开环聚合制备各种高性能材料,是一种先进的技术路线,是酚醛树脂高性能化的新途径,因此关于苯并恶嗪中间体的研究具有重要的价值和深刻的意义。本文主要研究悬浮法合成苯并恶嗪中间体工程学方面的内容。按小试、模型釜(冷、热模)试验、初步工程放大的思路进行阐述。 通过小试及模型釜(冷模试验),确定适合中间体合成的斜桨面三叶后掠式搅拌器与扁管挡板相搭配,搅拌器几何参数为:D/T=0.35~0.54,b/T=0.09,上翘角α=15°,后掠角β=45°,叶面倾角θ=35°;挡板数nB=3,挡板宽w=0.09T,离壁间隙C=(0.5~1.0)w,在湍流区可获得混合时间准数C1=N·tb<20,功率准数与流量准数之比Np/Nqd=4.11,搅拌特性属剪切型。 在40L釜中合成中间体,选择预聚阶段搅拌速度N1=60~80r/min,液-液分散期N2=200~250r/min,悬浮期N3=100~150 r/min时,可获得平均粒径为40目左右、粒径分布较窄,表面疏松多孔的球形中间体,各项性能(凝胶化时间、软化点、含酚率等)都达到预期指标,且反应过程稳定。 在模试釜试验基础上结合中间体反应的特点,针对反应的控制期(液-液分散期)确定工程放大准则为:单位体积功率恒定即Py=2.1~2.5Kw/m3;循环次数Nc>10次/分;放大后叶端线速度ND>1.00m/s且尽可能提高ND的值;同时预聚期均匀混合,悬浮期颗粒均匀悬浮。按此放大准则进行工程放大设计,搅拌器按部分几何参数相似,只调节D/T的值。1.0m3釜采用D/T=0.5,液-液分散期搅拌转速N2=111r/min=1.85r/s,叶端线速度:ND=1.11m/s。所设计的1.0m3釜已通过试车,运行正常,产品性能合格(凝胶化时间为2~4分/160±1℃,软化点108~121℃/落球法,含酚率<4.0%);颗粒平均粒径为30~40目,粒径分布窄,已形成300t/y的生产能力。5.0m3釜设计中采用D/T=045,液-液分散期搅拌转速N2=114r/min=1.90r/s,叶端线速度ND=1.54m/s。最后本文还研究了一种处理合成中间体工业中产生的大量含酚污水的方法—XDA-2大孔树脂吸附法,该法脱酚率高,投资少,操作简便。
【Abstract】 This paper focuses on the chemical engineering about benzoxazine intermediate suspension polymerization with phenol, formaldehyde, and aniline monomers. On the basis of experiments in model reactors, we can get the result that 3lade backswept inclined impellerlat pipe baffles are well applicable to the reaction, when the agitator diameter D=( 0. 350. 54)T, width b0. 09T, upward bending angle U =l5~ , backswept angleP4S0 , inclined angle of impeller face 0=150 ,and the baffle width w0.09T, the number of baffle n~3 ,the reaction is steady , the property of product is good, the average particle size of benzoxazine intermediate approximately 40 in. T is the reactors s inside diameter.The scalingp rule for the reactor of benzoxazine intermediate suspension polymerization is the power per volume P~2. 1?. 5Kw/rn3, the revolutions per minute N~>10 times/mm, the impeller tip speed ND>1.O m/s, in addition, in the process of pre-polymerization the reaction system must be well blended, and in the suspension process solid particles even suspended. According to the scalingp rule, 1. 0m3 and 5. 0m3 reactors are designed. In 1.0w3 reactor, D/T0.5, the stirrer speed of liquidiquid dispersion N2411r/min ; in 5.0w3 reactor D/T=O.45, N21 14r/min. 1. 0m3 reactor has been applied in the industry of benzoxazine intermediate, and works well, the yield per year is 300t. 5. Ow3 reactor is putting to use. This paper also studied phenol wastewater treatment in the industry of benzoxazine intermediateDA? resin adsorption method, it is an efficient and lowost way.
【Key words】 benzoxazine intermediate; suspension polymerization; chemical engineering; 3-blade backswept inclined impeller;
- 【网络出版投稿人】 四川大学 【网络出版年期】2002年 01期
- 【分类号】TQ252
- 【被引频次】8
- 【下载频次】287