响应面法优化双酚A甲醛酚醛树脂的合成研究
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摘要
以双酚A和甲醛为原料,正丁醇为溶剂,在对甲苯磺酸的催化作用下合成了双酚A甲醛酚醛树脂,着重探讨了反应温度、反应时间、催化剂用量和甲醛用量对游离甲醛含量的影响。研究结果表明:目标产物双酚A甲醛酚醛树脂成功制备。建立了游离甲醛含量的二次回归方程,同时使用响应面分析法中的BBD(Box-Behnken Design)对双酚A甲醛酚醛树脂的合成工艺进行优化,其最佳工艺条件为反应温度91℃、催化剂用量0.26 g、甲醛用量3.36 g和反应时间为6 h。
Bisphenol A formaldehyde phenolic resin was synthesized from 2,2-bis(4-hydroxyphenyl)propane(bisphenol A)and formaldehyde as raw materials,n-butanol as solvent and p-toluene sulfonic acid(TsOH)ascatalyst. The effects of reaction temperature,reaction time,catalyst dosage and formaldehyde dosage on freeformaldehyde content were emphatically discussed. The research results showed that the target product of bisphenolA formaldehyde phenolic resin was successfully prepared. The quadratic regression equation of free formaldehydecontent was established,and the synthesis process of bisphenol A formaldehyde phenolic resin was optimized byBBD(Box-Behnken Design) in response surface analysis. The optimum process conditions were reactiontemperature 91 ℃,catalyst dosage 0.26 g,formaldehyde dosage 3.36 g and reaction time 6 h.
Bisphenol A formaldehyde phenolic resin was synthesized from 2,2-bis(4-hydroxyphenyl)propane(bisphenol A)and formaldehyde as raw materials,n-butanol as solvent and p-toluene sulfonic acid(TsOH)ascatalyst. The effects of reaction temperature,reaction time,catalyst dosage and formaldehyde dosage on freeformaldehyde content were emphatically discussed. The research results showed that the target product of bisphenolA formaldehyde phenolic resin was successfully prepared. The quadratic regression equation of free formaldehydecontent was established,and the synthesis process of bisphenol A formaldehyde phenolic resin was optimized byBBD(Box-Behnken Design) in response surface analysis. The optimum process conditions were reactiontemperature 91 ℃,catalyst dosage 0.26 g,formaldehyde dosage 3.36 g and reaction time 6 h.
引文
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[3]薛祖源.双酚A生产工艺技术现状及展望[J].化工设计,2006,16(2):3-10.
[4]崔小明.国内外双酚A的供需现状及发展前景分析[J].石油化工技术与经济,2017,33(4):17-22.
[5]赵蕾.高耐热性酚醛环氧树脂的制备及其复合材料的性能研究[D].太原:中北大学,2017.
[6]张廷健,杨先贵,王公应,等.双酚S和双酚A与碳酸二苯酯共聚合成阻燃性聚碳酸酯[J].高分子材料科学与工程,2014,30(4):22-25.
[7]缪爱花,袁才登,姜东峰.双酚A型含氮酚醛树脂的合成及应用研究[J].热固性树脂,2003,18(1):18-20.
[8]葛成利,李枝芳,朱红军,等.高性能双酚A酚醛环氧树脂及其在覆铜板中应用[C].中国覆铜板技术市场研讨会,2015.
[9]LIN C T,LEE H T,CHEN J K. Synthesis andcharacterization of molybdenum/phenolic resin compositesbinding with aluminum nitride particles for diamondcutters[J].Applied Surface Science,2013,284:297-307.
[10]乔吉超,胡小玲,管萍.酚醛树脂胶粘剂的研究进展[J].中国胶粘剂,2006,15(7):45-48.
[11]马玉峰,王春鹏,许玉芝.酚醛树脂胶粘剂研究进展[J].粘接,2014,35(2):33-39.
[12]张天才,张凯,王永凤,等.聚醚胺/酚醛胺-环氧树脂体系的固化动力学研究[J].表面技术,2013,42(1):50-52.
[13]陈姝帆,李朗晨,洪海霞.环氧改性酚醛树脂的耐腐蚀性能研究[J].化工新型材料,2009,37(6):110-112;115.
[14]杜郢,周太炎,王哲,等.环氧改性酚醛树脂的合成与研究[J].石油化工,2012,41(5):583-587.
[15]全国人造板标准化技术委员会.木材胶粘剂及其树脂检验方法:GB/T 14074—2006[S].北京:中国标准出版社,2006.
[16]王雷,任新娟,高磊,等.降低可发泡性酚醛树脂中游离甲醛含量的研究[J].应用化工,2009,38(1):83-86.
[17]陈湘,蒋钧荣,陈建湘,等.双酚A型线性酚醛树脂的合成[J].热固性树脂,1999,14(3):10-13.
[18]GOTO K,HAYASHI S,SAITO T,et al. Epoxy resincomposition and prepreg made with the epoxy resincomposition:US20030135011[P].2003.
[19]TAGUCHI M,SUZUMURA Y,SAITOU T,et al. Flameretardant epoxy resin composition,and prepreg and fiber-reinforced composite materials made by using thecomposition:US20040034127[P].2004.
[20]HOOPER J R,STROTHERR K,FISH J,et al. Extremelylow viscosity materix epoxy suffusion resin system:US006040397[P].2000.
[21]TAKANO N,ARATA M,MURAI H,et al.Flame retardantepoxy resin composition for printed board,and prepreg andmetal foil clad laminate using the same:US6214 468 B1[P].2001.