机械活化干法制备新型淀粉基水泥砂浆保水增稠剂
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摘要
以木薯淀粉为原料,氯乙酸钠为醚化剂,三偏磷酸钠为交联剂,采用机械活化干法制备交联羧甲基淀粉保水剂。以取代度(the degree of substitution,DS)和黏度为评价指标,通过单因素和正交试验设计优化确定最佳制备工艺,采用红外光谱(fourier transform infrared spectroscopy,FTIR)、X-射线衍射(x-ray diffraction,XRD)、扫描电镜(scanning electron microscope,SEM)对交联羧甲基淀粉的结构进行表征,并考察不同添加量的交联羧甲基淀粉对水泥砂浆性能的影响。结果表明,交联羧甲基淀粉保水剂的最佳工艺参数为:淀粉与氯乙酸钠摩尔比为1∶0. 85、淀粉与氢氧化钠摩尔比为1∶1、淀粉质量1%的三偏磷酸钠、球磨温度50℃、球磨时间60 min,在此条件下制备的交联羧甲基淀粉取代度为0. 8373,黏度为3493 mPa·s。FTIR、XRD、SEM进一步证实木薯淀粉发生了交联羧甲基化反应。将0. 5%的交联羧甲基木薯淀粉添加到水泥砂浆中,砂浆的保水率从77. 1%提高到98. 2%,凝结时间由246 min延长至282 min,稠度值由57 mm减小至36 mm。微观测试表明,添加淀粉基保水剂的砂浆硬化体中方解石晶体减少,砂浆结构更加紧密。
By using cassava starch as raw materials,monochloroacetate as etherifying agent and sodium trimetaphosphate as cross-linking catalyst,the cross-linked carboxymethyl cassava starch was synthesized by mechanical activation-strengthened dry method. Single factor experiments and orthogonal array design methods were used to optimize the preparation conditions based on the degree of substitution (DS) and the viscosity. The structure of the cross-linked carboxymethyl cassava starch were characterized by using fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscope (SEM). The cross-linked carboxymethyl cassava starch was then applied to cement mortar.The optimal process parameters were obtained as follows: the mole ratio of starch and sodium chloracetate was 1∶ 0. 85. The mole ratio of starch and sodium hydroxide was 1∶ 1. The sodium trimetaphosphate of the starch weight was 1%,ball-milling temperature was 50 ℃. Ball-milling time was 60 min. The degree of substitution of products was 0. 8373. And the viscosity of products was 3493 mPa·s. The cross-linking and etherification reaction of cassava starch have been further confirmed by FTIR,XRD,SEM. By adding the 0. 5% of cross-linked carboxymethyl cassava starch to the cement mortar,the water-retention rate of the cement mortar increased from 77. 1% to 98. 2%,the setting time prolonged from 246 min to 282 min,and the consistency decreased from 57 mm to 36 mm. Microscopic test showed that the calcite crystal of cement mortar mixed with appropriate cross-linked carboxymethyl cassava starch was decreased,and the cementitious materials exhibited more intensive structure.
By using cassava starch as raw materials,monochloroacetate as etherifying agent and sodium trimetaphosphate as cross-linking catalyst,the cross-linked carboxymethyl cassava starch was synthesized by mechanical activation-strengthened dry method. Single factor experiments and orthogonal array design methods were used to optimize the preparation conditions based on the degree of substitution (DS) and the viscosity. The structure of the cross-linked carboxymethyl cassava starch were characterized by using fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscope (SEM). The cross-linked carboxymethyl cassava starch was then applied to cement mortar.The optimal process parameters were obtained as follows: the mole ratio of starch and sodium chloracetate was 1∶ 0. 85. The mole ratio of starch and sodium hydroxide was 1∶ 1. The sodium trimetaphosphate of the starch weight was 1%,ball-milling temperature was 50 ℃. Ball-milling time was 60 min. The degree of substitution of products was 0. 8373. And the viscosity of products was 3493 mPa·s. The cross-linking and etherification reaction of cassava starch have been further confirmed by FTIR,XRD,SEM. By adding the 0. 5% of cross-linked carboxymethyl cassava starch to the cement mortar,the water-retention rate of the cement mortar increased from 77. 1% to 98. 2%,the setting time prolonged from 246 min to 282 min,and the consistency decreased from 57 mm to 36 mm. Microscopic test showed that the calcite crystal of cement mortar mixed with appropriate cross-linked carboxymethyl cassava starch was decreased,and the cementitious materials exhibited more intensive structure.
引文
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[17]陈渊,黄祖强,杨家添,等.机械活化预处理甘蔗渣制备醋酸纤维素的工艺[J].农业工程学报,2010,26(9):374-380.
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[22]谢秋季,晏全,杨家添,等.机械活化干法制备玉米羧甲基淀粉工艺研究[J].食品工业科技,2017,38(10):236-241.
[23]佘艳,张光旭,鄢烈祥,等.交联-羧甲基淀粉合成工艺可视化优化的研究[J].中国粮油学报,2009,24(4):62-65.
[24]郭庆兴,童群义.交联羟丙基羧甲基木薯淀粉性质的研究[J].食品工业科技,2012,33(23):122-124,128.
[25]住房和城乡建设部.建筑砂浆基本性能试验方法JGJ/T 70-2009[S].北京:中国建筑工业出版社,2009.
[26]谭义秋,黄祖强,农克良.高取代度木薯羧甲基淀粉的合成及表征[J].过程工程学报,2010(1):173-178.
[27]张筱璐,万冰清,刘丽丽,等.溶剂法制备高粘度羧甲基淀粉[J].华东理工大学学报(自然科学版),2007,33(3):365-368.
[28]徐忠,周美琴,杨成.交联淀粉的制备工艺研究[J].食品科学,2008,29(8):194-196.
[29]谭义秋,黄祖强,农克良.机械活化木薯淀粉羧甲基化产物糊性质的研究(Ⅱ)[J].食品科学,2011,32(15):30-33.
[30]许晖,孙兰萍,赵大庆,等.马铃薯交联淀粉的制备与结构表征[J].中国粮油学报,2007,22(5):68-72.
[31]韩琼洁,张斌,倪群玉.交联木薯淀粉的制备及性能[J].东华大学学报,2016,42(1):58-61.
[32]谢慧东,槐衍廷,张勇,等.改性玉米秸秆纤维素在砂浆中的应用研究[J].新型建筑材料,2015,42(5):4-7,39.
[33]郭和平.干粉砂浆中常用添加剂及作用[J].山西建筑,2009,35(2):176-177.
[34]朱宪荣,李晓生,张循海,等.改性糯米淀粉对砂浆性能的影响[J].高师理科学刊,2012,32(2):69-72.
[35]Yang F W,Zhang B J,Ma Q L.Study of sticky rice-lime mortar technology for there storation of historical masonry construction[J].Accounts of Chemical Reseaech,2010,43(6):936-944.
[2]詹镇峰,李从波,陈文钊.纤维素醚的结构特点及对砂浆性能的影响[J].混凝土,2009(10):110-112.
[3]王培铭,赵国荣,张国防.纤维素醚在新拌砂浆中保水增稠作用及其机理[J].硅酸盐学报,2017,45(8):1190-1196.
[4]张冠伦,王玉吉,孙振平.混凝土外加剂原理与应用[M].北京:中国建筑出版社,1982.
[5]鞠丽艳,张雄.建筑砂浆保水增稠剂的性能及作用机理[J].建筑材料学报,2003,6(1):25-29.
[6]Brouillet F,Bataile B,Cartilier L.High-amylose sodium carboxymethyl starch matrices for oral susained drug-release:formulation aspects and in vitro drug-release evaluation[J].Iternational Journal of Pharmaceutics,2008,356(1-2):52-60.
[7]Ghanshyam S C,Saroj C J,Monika V.Post functionalization of carboxymethylated starch and acrylonitrile sased networks through amidoximation for use as ion sorbents[J].Carbohydrate Polymers,2006,66(4):435-443.
[8]沈文忠,张雄.羧甲基淀粉对于建筑砂浆性能的影响[J].化学建材,2004(6):49-50.
[9]金惠平.高粘度交联羧甲基淀粉的研究[J].中国食品添加剂,2004(6):26-28.
[10]Ragheb A A,El-ssyiad H S,Hebeish A P.Preparation and charaeterization of carboxyethyl stareh(CMS)produets and their utilizationin textile printing[J].Stareh/Starke,1997,49(6):238-245.
[11]Anirudhan T S,Parvathy J.Novel semi-IPN based on crosslinked carboxymethyl starch and clay for the in vitro release of theophylline[J].International Journal of Biological Macromolecules,2014,67:238-245.
[12]张运芳,钟耕,钟春生,等.快速崩解羧甲基-交联玉米淀粉性能研究及结构表征[J].中国粮油学报,2009,24(8):74-79.
[13]陈振华,陈鼎.机械合金化与固液反应球磨[M].北京:化学工业出版社,2005:492.
[14]Huang Z Q,Lu J P,Li X H,et al.Effect of mechanical activation on physico-chemical properties and structure of cassava starch[J].Carbohydrate Polymers,2007,68(1):128-135.
[15]黄祖强,陈渊,钱维金,等.机械活化对玉米淀粉结晶结构与化学反应活性的影响[J].化工学报,2007,58(5):1307-1313.
[16]黄祖强,陈渊,钱维金,等.机械活化对木薯淀粉醋酸酯化反应的强化作用[J].过程工程学报,2007,7(3):501-505.
[17]陈渊,黄祖强,杨家添,等.机械活化预处理甘蔗渣制备醋酸纤维素的工艺[J].农业工程学报,2010,26(9):374-380.
[18]廖政达,张燕娟,文胜.机械活化木薯酒糟液化物合成树脂的FT-IR表征[J].化工新型材料,2012,40(3):60-62.
[19]陈渊,杨家添,黄祖强,等.机械活化固相化学反应制备木薯醋酸酯淀粉[J].食品与发酵工业,2013,39(7):135-141.
[20]Hu H Y,Liu W D,Shi J,et al.Structure and functional properties of octenyl succinic anhydride modified starch prepared by a non-conventional technology[J].Starch/Starke,2016,68(1-2):151-159.
[21]陈渊,杨家添,谢秋季,等.木薯羧甲基淀粉的机械活化固相化学法制备、表征及其特性[J].食品科学,2018,39(2):45-52.
[22]谢秋季,晏全,杨家添,等.机械活化干法制备玉米羧甲基淀粉工艺研究[J].食品工业科技,2017,38(10):236-241.
[23]佘艳,张光旭,鄢烈祥,等.交联-羧甲基淀粉合成工艺可视化优化的研究[J].中国粮油学报,2009,24(4):62-65.
[24]郭庆兴,童群义.交联羟丙基羧甲基木薯淀粉性质的研究[J].食品工业科技,2012,33(23):122-124,128.
[25]住房和城乡建设部.建筑砂浆基本性能试验方法JGJ/T 70-2009[S].北京:中国建筑工业出版社,2009.
[26]谭义秋,黄祖强,农克良.高取代度木薯羧甲基淀粉的合成及表征[J].过程工程学报,2010(1):173-178.
[27]张筱璐,万冰清,刘丽丽,等.溶剂法制备高粘度羧甲基淀粉[J].华东理工大学学报(自然科学版),2007,33(3):365-368.
[28]徐忠,周美琴,杨成.交联淀粉的制备工艺研究[J].食品科学,2008,29(8):194-196.
[29]谭义秋,黄祖强,农克良.机械活化木薯淀粉羧甲基化产物糊性质的研究(Ⅱ)[J].食品科学,2011,32(15):30-33.
[30]许晖,孙兰萍,赵大庆,等.马铃薯交联淀粉的制备与结构表征[J].中国粮油学报,2007,22(5):68-72.
[31]韩琼洁,张斌,倪群玉.交联木薯淀粉的制备及性能[J].东华大学学报,2016,42(1):58-61.
[32]谢慧东,槐衍廷,张勇,等.改性玉米秸秆纤维素在砂浆中的应用研究[J].新型建筑材料,2015,42(5):4-7,39.
[33]郭和平.干粉砂浆中常用添加剂及作用[J].山西建筑,2009,35(2):176-177.
[34]朱宪荣,李晓生,张循海,等.改性糯米淀粉对砂浆性能的影响[J].高师理科学刊,2012,32(2):69-72.
[35]Yang F W,Zhang B J,Ma Q L.Study of sticky rice-lime mortar technology for there storation of historical masonry construction[J].Accounts of Chemical Reseaech,2010,43(6):936-944.
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