选择性氧化法合成双醛纤维素硫酸酯
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摘要
为了发展一个新的生物活性物质利用纤维素资源,采用高碘酸钠(NalO4)对微晶纤维素(MCC)进行选择性氧化,又与亚硫酸氢钠(NaHSO3)进行磺化反应,得到了双醛纤维素硫酸酯(OSC)。通过红外光谱(FTIR)分析手段对产品结构进行了表征。并考察了工艺参数对DAC醛基含量和OSC取代度的影响,得出了各合成阶段的关键工艺参数——时间、温度、pH值和反应物配比的最佳控制值。结果表明:当反应物配比为n(NaHSO3)∶n(DAC)=2∶1,产品合成温度为22℃,合成时间为2 h时,所得产品磺酸基取代度最高,并具有明显的表面活性。
In order to develop a novel bioactive material utilizing cellulose resource, dialdehyde cellulose sulphate(OSC) was synthesized by oxidizing microcrystal cellulose with sodium periodate followed by the sulfonation reaction with sodium bisulfite. The structure of OSC was characterized by means of FT-IR. The effects of process parameter on the aldehyde groop content and the degree of substitution were investigated. The optimum control value of the critic parameter-time, temperature, pH and reactants ratio of every stage were got. The results showed that the ideal sulfonated cellulose could be prepared when the mole ratios of n(NaHSO3): n(DAC)=2:1, reacting 2 h and at 22 ℃, the OSC has good surface activity.
In order to develop a novel bioactive material utilizing cellulose resource, dialdehyde cellulose sulphate(OSC) was synthesized by oxidizing microcrystal cellulose with sodium periodate followed by the sulfonation reaction with sodium bisulfite. The structure of OSC was characterized by means of FT-IR. The effects of process parameter on the aldehyde groop content and the degree of substitution were investigated. The optimum control value of the critic parameter-time, temperature, pH and reactants ratio of every stage were got. The results showed that the ideal sulfonated cellulose could be prepared when the mole ratios of n(NaHSO3): n(DAC)=2:1, reacting 2 h and at 22 ℃, the OSC has good surface activity.
引文
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[8]Huang Fengyu.Synthesis and Application of Concrete Water Reducers Based on Natural Polymers[D].Dalian University of Technology,2008(6):24-25.
[2]Xiong J,Ye J,He X,et al.The improved heterogeneous reaction of the oxidation of cellulose by periodic[J].Polym.Mater.Sci.Eng.,2000,16(3):172-175.
[3]Vicini S,Princi E,Luciano G,et al.Thermal analysis and characterisation of cellulose oxidised with sodium methaperiodate[J].Thermochim.Acta,2004,418(1-2):123-130.
[4]Dash Rajalaxmi,Nan Jiang,Gelbaum Leslie.Synthesis of novel water-soluble sulfonated celluloses[J].Carbohydrate Research,2010,345:284-290.
[5]Jianguo Zhang,Nan Jiang,Zheng Dang.Oxidation and sulfonationcellulosics[J].Cellulose,2008,15:489-496.
[6]Kurbanjian Rouzi(库尔班江·肉孜),Halidan Mamat(哈丽丹·买买提),Alimujiang(阿里木江),阿金沙.Synthesis and dispersing mechanism of cellulose sulfonate as a water—reducing agent for cement[J].Concrete(混凝土),2011,7:69-73.
[7]FengYa-qing(冯亚青),LIU Yan(刘燕),ZHANG Xiaodong(张晓东),et al.Prepration of Dialdehyde cellulose and Its Absorption Propity[J].Journal of Tianjin University,2002,35(6):766-768.
[8]Huang Fengyu.Synthesis and Application of Concrete Water Reducers Based on Natural Polymers[D].Dalian University of Technology,2008(6):24-25.