间苯二酚-双醛淀粉-甲醛共缩聚树脂胶黏剂制备
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摘要
以玉米淀粉为原料,通过高碘酸钠在酸性条件下氧化得到双醛淀粉。将双醛淀粉与甲醛一起作为醛基给予体,与间苯二酚(R)共缩聚制备间苯二酚-双醛淀粉-甲醛(RDSF)树脂胶黏剂。研究了双醛淀粉用量、共反应p H、共反应温度和共反应时间对RDSF树脂胶黏剂固体含量、黏度、固化时间和胶接强度的影响。结果表明,双醛淀粉加入量为0. 15mol,共反应p H值为9. 0,共反应温度为70℃,共反应时间为90 min时,制得的RDSF树脂胶黏剂综合性能最佳,此时固体含量为42. 59%,黏度为725 m Pa·s,固化时间为53 s,干状胶合强度为1. 38 MPa,湿状胶合强度为1. 17 MPa。傅里叶变换红外光谱测试发现RDSF树脂的结构近似于间苯二酚-甲醛(RF)树脂,表明RDSF树脂可代替RF树脂使用。差示扫描量热分析发现RDSF树脂的固化温度和固化焓值低于RF树脂,固化峰值温度为77. 43℃,固化焓值为-238. 91 J/g,表明其固化能耗更低。
Dialdehyde starch was obtained by raw material corn starch oxidized with sodium periodate under acid condition. The resorcinol-dialdehyde starch-formaldehyde( RDSF) resin adhesive was prepared by resorcinol( R) copolycondensation with aldehyde donor of dialdehyde starch and formaldehyde. The effects of dialdehyde starch content,copolycondensation pH,copolycondensation temperature and copolycondensation time on solid content,viscosity,curing time and bonding strength of RDSF resin adhesive were studied. The results show that RDSF resin adhesive has the best comprehensive performance when the dialdehyde starch content is 0. 15 mol,copolycondensation pH is 9,copolycondensation temperature is 60 ℃ and copolycondensation time is 90 min. At this time,the solid content is 42. 59%,the viscosity is 725 m Pa·s,the curing time is 53 s,the dry bonding strength is 1. 38 MPa,and the wet bonding strength is1. 17 MPa. The FT-IR results show that the structure of RDSF resin is similar to that of resorcinol formaldehyde( RF)resin,which indicating that RDSF resin could be used instead of RF resin. DSC analysis shows that the curing temperature and curing enthalpy of RDSF resin are lower than those of RF resin,the peak curing temperature is 77. 43 ℃ and the enthalpy of curing is-238. 91 J/g,indicating that the curing energy consumption of RDSF resin is lower.
Dialdehyde starch was obtained by raw material corn starch oxidized with sodium periodate under acid condition. The resorcinol-dialdehyde starch-formaldehyde( RDSF) resin adhesive was prepared by resorcinol( R) copolycondensation with aldehyde donor of dialdehyde starch and formaldehyde. The effects of dialdehyde starch content,copolycondensation pH,copolycondensation temperature and copolycondensation time on solid content,viscosity,curing time and bonding strength of RDSF resin adhesive were studied. The results show that RDSF resin adhesive has the best comprehensive performance when the dialdehyde starch content is 0. 15 mol,copolycondensation pH is 9,copolycondensation temperature is 60 ℃ and copolycondensation time is 90 min. At this time,the solid content is 42. 59%,the viscosity is 725 m Pa·s,the curing time is 53 s,the dry bonding strength is 1. 38 MPa,and the wet bonding strength is1. 17 MPa. The FT-IR results show that the structure of RDSF resin is similar to that of resorcinol formaldehyde( RF)resin,which indicating that RDSF resin could be used instead of RF resin. DSC analysis shows that the curing temperature and curing enthalpy of RDSF resin are lower than those of RF resin,the peak curing temperature is 77. 43 ℃ and the enthalpy of curing is-238. 91 J/g,indicating that the curing energy consumption of RDSF resin is lower.
引文
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[3] Zhang Y,Gu J,Tan H,et al. Straw based particleboard bonded with composite adhesives[J]. BioResources,2011,6:464-476.
[4]王春鹏,赵临五.酚醛树脂胶黏剂的改性[J].林产化学与工业,1999,19(2):77-81.Wang C P,Zhao L W. Modification of phenolic resin adhesives[J].Chemistry and industry of forest products,1999,19(2):77-81.
[5] Alamsyah E M,Yamada M,Taki K. Bondability of tropical fastgrowing tree species III:curing behavior of resorcinol formaldehyde resin adhesive at room temperature and effects of extractives of Acacia mangium wood on bonding[J]. J. Wood Sci.,2008,54:208-213.
[6]陈志安,刘书林,郭俊英,等.响应面优化法研究果糖间苯二酚树脂胶粘剂的合成[J].高分子材料科学与工程,2012,28(10):8-11.Chen Z A,Liu S L,Guo J Y,et al. Optimization for synthesis of fructose-resorcinol resin adhesive by response surface methodology[J]. Polymer Materials Science&Engineering,2012,28(10):8-11.
[7] Wongsagon R,Shobsngob S,Varavinit S. Preparation and physicochemical properties of dialdehyde tapioca starch[J]. Starch/St?rke,2005,57:166-172.
[8] Mu C,Liu F,Cheng Q,et al. Collagen cryogel cross-linked by dialdehyde starch[J]. Macromol. Mater. Eng.,2010,295:100-107.
[9] Zhang L,Zhang S,Dong F,et al. Antioxidant activity and in vitro digestibility of dialdehyde starches as influenced by their physical and structural properties[J]. Food Chem.,2014,149:296-301.
[10] Zhang Y,Ding L,Gu J,et al. Preparation and properties of a starch-based wood adhesive with high bonding strength and water resistance[J]. Carbohydr. Polym.,2015,115:32-37.
[11] Zuo Y,Liu W,Xiao J,et al. Preparation and characterization of dialdehyde starch by one-step acid hydrolysis and oxidation[J]. Int.J. Biol. Macromol.,2017,103:1257-1264.
[12] Yu L,Dean K,Li L. Polymer blends and composites from renewable resources[J]. Prog. Polym. Sci.,2006,31:576-602.
[13] Alma M H,Basturk M A. Liquefaction of grapevine cane(Vit is vinisera L.)waste and its application to phenol-formaldehyde type adhesive[J]. Ind. Crops Prod.,2006,24:171-176.
[14] Kamke F A,Lee J N. Adhesive penetration in wood—a review[J].Wood Fiber Sci.,2007,39:205-220.
[15] Zombort B G,Kamke F A,Watson L T. Simulation of the internal conditions during the hot-pressing process[J]. Wood Fiber Sci.,2007,35:2-23.
[16]王洪府.固体多聚甲醛制备酚醛树脂及其发泡工艺研究[D].武汉:武汉理工大学,2012.Wang H F. Preparation of phenolic resin from solid polyformaldehyde and its foaming process[D]. Wuhan:Wuhan University of Technology,2012.
[17]肖俊华,左迎峰,刘文杰,等.秸秆人造板用胶黏剂研究进展[J].材料导报,2016,30(17):78-83.Xiao J H,Zuo Y F,Liu W J,et al. Research progress of adhesives for strawboard[J]. Materials Review,2016,30(17):78-83.
[18]张云云,张一帆.黏度对酚醛浸渍树脂润湿性能的影响[J].中国胶粘剂,2006,15(1):11-14.Zhang Y Y,Zhang Y F. The influence of viscosity to phenol-formaldehyde impregnated resin's wettability[J]. China Adhesives,2006,15(1):11-14.