橡胶硫化促进剂M新型精制工艺研究
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摘要
使用溶解-重结晶法,对溶剂法精制橡胶硫化促进剂M的工艺进行探索及优化。首先考察不同溶剂在不同温度下对粗M中树脂的分离效果,以此找到最佳的分离溶剂;在最佳分离溶剂的基础上,探索多段实验对分离效果的影响。实验结果表明,甲苯和异丙醇的最佳分离温度皆在各自的沸点附近;在最佳m(粗M)∶m(甲苯)下,多段实验的分离效果明显好于单段实验;产率可达到61.2%~67.4%,熔点范围为181.2~181.6℃。因此,选用甲苯和异丙醇作溶剂,结合多段分离,可以明显提高分离效果。
The new process of solvent refining rubber vulcanization accelerator M was explored and optimized by using the method of dissolution-recrystallization.In order to find the best separation of solvent,the different solvents at different temperatures on the separation effect of coarse M were examined.Then multi-stage experiments' influence on the separation effect was explored based on the optimal separation solvent.The experimental results showed that the best separation temperature of benzene and isopropyl alcohol was in the vicinity of the boiling point respectively.Under the optimum m(coarse M)∶m(toluene)ratio,multi-stage experiment separation effect was obviously better than that of single-stage experiments.The production yield could be reached 61.2%~67.4%,the range of melting points was 181.2~181.6℃.Therefore,the selection of toluene and isopropyl alcohol as solvent,combined with multi-stage separation,can significantly improve the separation efficiency.
The new process of solvent refining rubber vulcanization accelerator M was explored and optimized by using the method of dissolution-recrystallization.In order to find the best separation of solvent,the different solvents at different temperatures on the separation effect of coarse M were examined.Then multi-stage experiments' influence on the separation effect was explored based on the optimal separation solvent.The experimental results showed that the best separation temperature of benzene and isopropyl alcohol was in the vicinity of the boiling point respectively.Under the optimum m(coarse M)∶m(toluene)ratio,multi-stage experiment separation effect was obviously better than that of single-stage experiments.The production yield could be reached 61.2%~67.4%,the range of melting points was 181.2~181.6℃.Therefore,the selection of toluene and isopropyl alcohol as solvent,combined with multi-stage separation,can significantly improve the separation efficiency.
引文
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[6]吴志庆.促进剂M合成及树脂处理工艺条件改进[J].科技创新与应用,2015(9):42.
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[9]徐承秋,吴艳萍,薛香菊,等.橡胶硫化促进剂MBT的精制工艺:102718728A[P].2012-10-10.
[10]杜孟成,王文博,魏成磊,等.硫化促进剂2-巯基苯并噻唑的纯化工艺:101693701A[P].2010-04-14.
[11]PRAKORN RAMAKUL,MILAN HRONEC,URA PANCHAROEN.Purification of 2-mercaptobenzothiazole by solvent extraction[J].Korean Journal of Chemical Engineering,2007,24(3):82-287.
[12]范德兴.影响熔点测定结果的因素[J].化学世界,1985(5):187-188.
[13]余新武.复分解反应法制备普鲁士蓝溶胶[J].黄石师院学报(自然科学报),1984(1):79-82.
[2]朱继琴,李景宁.2-巯基苯并噻唑衍生物的合成进展[J].化学通报,2009(8):681-686.
[3]许春华.中国橡胶工业原材料和工艺技术的绿色化进展[J].橡塑技术与装备,2013,39(1):10-20.
[4]RAIKIEIVICZ MARIN,LIESLAK ROMAN,TURLINSKI ZDZISLAW,et a1.Manufacture of master batch formulations as solid additives for rubber compounds:181468[P].2001-07-03.
[5]MAKOTO SUGAHARA,NISHINOMIYA,KENJIRO MORI.Process for the rapid production of 2-mercaptobenzothiazole:3818025[P].1967-06-18.
[6]吴志庆.促进剂M合成及树脂处理工艺条件改进[J].科技创新与应用,2015(9):42.
[7]安静.橡胶硫化促进剂MBT的提纯方法:102827101A[P].2012-12-19.
[8]王树华,王树领,王树恒,等.橡胶硫化促进剂MBT的精制方法:101108834[P].2009-03-18.
[9]徐承秋,吴艳萍,薛香菊,等.橡胶硫化促进剂MBT的精制工艺:102718728A[P].2012-10-10.
[10]杜孟成,王文博,魏成磊,等.硫化促进剂2-巯基苯并噻唑的纯化工艺:101693701A[P].2010-04-14.
[11]PRAKORN RAMAKUL,MILAN HRONEC,URA PANCHAROEN.Purification of 2-mercaptobenzothiazole by solvent extraction[J].Korean Journal of Chemical Engineering,2007,24(3):82-287.
[12]范德兴.影响熔点测定结果的因素[J].化学世界,1985(5):187-188.
[13]余新武.复分解反应法制备普鲁士蓝溶胶[J].黄石师院学报(自然科学报),1984(1):79-82.