挤压膨化机无碱制备氧化淀粉及其机理研究
摘要
本文借鉴机械力化学理论，利用挤压膨化机的高温、强剪切力的作用对淀粉亚颗粒“膜”、“带或壁”的破坏作用和对淀粉晶体位错作用，提高反应试剂与淀粉分子混合度，增加和内移的淀粉化学活性点，突破干法生产变性淀粉存在化学试剂和淀粉混合不均匀、产品溶解性差等技术难题，确立了一种新型无碱干法生产氧化淀粉工艺。通过采用XRD、DSC、SEM、ATR-FTIR、1H NMR等先进分析手段，揭示了挤压膨化机无碱制备氧化淀粉的机理。主要研究结果如下：
(1)制备条件对氧化淀粉氧化度及水溶指数的影响：高温或低水分均会降低挤压机的强剪切力对淀粉分子间作用力的破坏作用。高转速有助于破坏淀粉晶体结构，促进淀粉分子和化学试剂的混合，提高反应均匀性；但因高转速缩短了物料在套筒保留时间，故其氧化淀粉羧基含量有所降低。响应面方差分析，各反应条件之间存在显著性不同的交互作用。NaClO和H2O2在挤压膨化机中的存在状态以及沸点不同，导致制备两种氧化淀粉的最优反应条件不同。
(2)淀粉氧化后生成的羧基由于其亲水性和电荷的排斥作用，水溶指数不断上升，凝沉性下降，特征粘度、回凝比率下降，热稳定性增强（崩解比率达到了2.73%）。
(3)与湿法制备的氧化淀粉和商品羟丙基交联淀粉比较，本试验工艺制备氧化淀粉的膜，拉伸强度极大（19.39MPa）；但由于分子链比较短，所以断裂伸长率比较低（13.61%）。该法制备的氧化淀粉膜可用于制备高强度的可降解膜材料。
(4)挤压膨化机无碱制备氧化淀粉的机理：挤压膨化机高温强剪切作用使淀粉机械力化学的活性点增多和深入颗粒内部，显著提高了反应均匀性。同时挤压膨化机高温强剪切作用使大量淀粉分子中C-O-C以氧化脱水的形式断裂，断裂后生成自由基，从而提高了挤压膨化机的反应效率。此外，挤压膨化机高温强剪切作用还可通过影响D-吡喃葡萄糖环的构型，活化淀粉。
(5)不同氧化剂对淀粉的氧化方式不同。氧化能力最强的ClO2羰基含量最高、羧基含量最低、其他理化性质也较差；H2O2氧化使淀粉剧烈降解，各项理化性质均比ClO2好，缺点是颜色较深；NaClO在挤压机内以小颗粒的形式存在，高温强剪切作用不能破坏NaClO颗粒，制备氧化淀粉的羧基含量最高。催化剂不仅能促进了羰基和羧基的生成和淀粉分子进一步裂解，但同时也会加快双氧水的分解。
In the present study, according to mechanochemistry theory, the high temperature, strongshear stress of screw extruder damaged the film, ribbon and wall of sub-granule, and madestarch crystals be dislocated. Thus reaction reagents were mixed homogeneously with starchmolecules, meanwhile chemical activity sites on starch molecules increased and shifted insidestarch granules. This work had broken some technical problems for wide application of drymethod for preparing modified starch, such as inhomogeneous mixing of starch and reactionreagents, poor sulubility of oxidized starch and so on. So preparation of oxidized starch byreactive extrusion under alkali-free conditions could be described as a new dry technology.This study also used some latest research tools to study mechanism of preparing oxidizedstarch in a screw extruder under alkali-free conditions, such as DSC, SEM, XRD, NMR,ATR-FTIR and so on. The main research contents were as follows:
(1) The effects of extrusive condition on the carboxyl content (CC) and water solubilityindex (WSI) of oxidized corn starch were found out clearly. High temperature or low watercontent reduced mechanical force on starch. Increasing screw speed increased the extent ofstarch shear-induced degradation and promoted the uniformity of mixing starch with oxidantand water. However, increasing screw speed would reduce mean residence time in theextruder, the carboxyl content of oxidized starch was not promoted with the increase of screwspeed. NaClO and H2O2in the extruder had different state and boiling points, resulting indifferent optimal reaction conditions for preparing two kinds of oxidized starch.
(2) Due to hydrophilicity and charge repulsion of oxidized starch, its solubility andthermal stability rose up, and its retrogradation and intrinsic viscosity decreased.
(3) Oxidized starch prepared by this method could be used as materials for preparing high-strength degradable films, because it's molecular chain stretched. Elongation at break of filmsprepared by this oxidized starch was poor (13.61%), because its molecular weight was small.
(4) The mechanism of preparing oxidized starch in a screw extruder under alkali-freeconditions were found out. The high temperature, strong shear stress of screw extruder madechemical activity sites increase and shift inside starch granules, which improved distributionuniformity of functional groups in starch granules. And screw extruder also broke a lot of C- O-C, which made starch molecules generate free radical, so reaction efficiency was improved.Moreover, the strong shear stress of screw extruder could activate starch by changing D-glucopyranosyl ring configuration.
(5) Different oxidants had different forms of oxidizing starch. Oxidation of ClO2is thestrongest, but oxidized starch prepared using it has the most carbonyl content, the leastcarboxyl content and poor physical and chemical properties. H2O2made starch degradeseverely. Oxidized starch prepared using H2O2had good physical and chemical properties, butpoor color. NaClO in the extrude existed in the form of small particles, and high temperatureand strong shearing did not destroy NaClO particles. Oxidized starch prepared using NaClOhas the most carboxyl content. Catalyst made oxidized starch had more carbonyl and carboxylgroups, and degraded starch molecules heavily. Meanwhile catalyst accelerated thedecomposition of hydrogen peroxide.
(1)制备条件对氧化淀粉氧化度及水溶指数的影响：高温或低水分均会降低挤压机的强剪切力对淀粉分子间作用力的破坏作用。高转速有助于破坏淀粉晶体结构，促进淀粉分子和化学试剂的混合，提高反应均匀性；但因高转速缩短了物料在套筒保留时间，故其氧化淀粉羧基含量有所降低。响应面方差分析，各反应条件之间存在显著性不同的交互作用。NaClO和H2O2在挤压膨化机中的存在状态以及沸点不同，导致制备两种氧化淀粉的最优反应条件不同。
(2)淀粉氧化后生成的羧基由于其亲水性和电荷的排斥作用，水溶指数不断上升，凝沉性下降，特征粘度、回凝比率下降，热稳定性增强（崩解比率达到了2.73%）。
(3)与湿法制备的氧化淀粉和商品羟丙基交联淀粉比较，本试验工艺制备氧化淀粉的膜，拉伸强度极大（19.39MPa）；但由于分子链比较短，所以断裂伸长率比较低（13.61%）。该法制备的氧化淀粉膜可用于制备高强度的可降解膜材料。
(4)挤压膨化机无碱制备氧化淀粉的机理：挤压膨化机高温强剪切作用使淀粉机械力化学的活性点增多和深入颗粒内部，显著提高了反应均匀性。同时挤压膨化机高温强剪切作用使大量淀粉分子中C-O-C以氧化脱水的形式断裂，断裂后生成自由基，从而提高了挤压膨化机的反应效率。此外，挤压膨化机高温强剪切作用还可通过影响D-吡喃葡萄糖环的构型，活化淀粉。
(5)不同氧化剂对淀粉的氧化方式不同。氧化能力最强的ClO2羰基含量最高、羧基含量最低、其他理化性质也较差；H2O2氧化使淀粉剧烈降解，各项理化性质均比ClO2好，缺点是颜色较深；NaClO在挤压机内以小颗粒的形式存在，高温强剪切作用不能破坏NaClO颗粒，制备氧化淀粉的羧基含量最高。催化剂不仅能促进了羰基和羧基的生成和淀粉分子进一步裂解，但同时也会加快双氧水的分解。
In the present study, according to mechanochemistry theory, the high temperature, strongshear stress of screw extruder damaged the film, ribbon and wall of sub-granule, and madestarch crystals be dislocated. Thus reaction reagents were mixed homogeneously with starchmolecules, meanwhile chemical activity sites on starch molecules increased and shifted insidestarch granules. This work had broken some technical problems for wide application of drymethod for preparing modified starch, such as inhomogeneous mixing of starch and reactionreagents, poor sulubility of oxidized starch and so on. So preparation of oxidized starch byreactive extrusion under alkali-free conditions could be described as a new dry technology.This study also used some latest research tools to study mechanism of preparing oxidizedstarch in a screw extruder under alkali-free conditions, such as DSC, SEM, XRD, NMR,ATR-FTIR and so on. The main research contents were as follows:
(1) The effects of extrusive condition on the carboxyl content (CC) and water solubilityindex (WSI) of oxidized corn starch were found out clearly. High temperature or low watercontent reduced mechanical force on starch. Increasing screw speed increased the extent ofstarch shear-induced degradation and promoted the uniformity of mixing starch with oxidantand water. However, increasing screw speed would reduce mean residence time in theextruder, the carboxyl content of oxidized starch was not promoted with the increase of screwspeed. NaClO and H2O2in the extruder had different state and boiling points, resulting indifferent optimal reaction conditions for preparing two kinds of oxidized starch.
(2) Due to hydrophilicity and charge repulsion of oxidized starch, its solubility andthermal stability rose up, and its retrogradation and intrinsic viscosity decreased.
(3) Oxidized starch prepared by this method could be used as materials for preparing high-strength degradable films, because it's molecular chain stretched. Elongation at break of filmsprepared by this oxidized starch was poor (13.61%), because its molecular weight was small.
(4) The mechanism of preparing oxidized starch in a screw extruder under alkali-freeconditions were found out. The high temperature, strong shear stress of screw extruder madechemical activity sites increase and shift inside starch granules, which improved distributionuniformity of functional groups in starch granules. And screw extruder also broke a lot of C- O-C, which made starch molecules generate free radical, so reaction efficiency was improved.Moreover, the strong shear stress of screw extruder could activate starch by changing D-glucopyranosyl ring configuration.
(5) Different oxidants had different forms of oxidizing starch. Oxidation of ClO2is thestrongest, but oxidized starch prepared using it has the most carbonyl content, the leastcarboxyl content and poor physical and chemical properties. H2O2made starch degradeseverely. Oxidized starch prepared using H2O2had good physical and chemical properties, butpoor color. NaClO in the extrude existed in the form of small particles, and high temperatureand strong shearing did not destroy NaClO particles. Oxidized starch prepared using NaClOhas the most carboxyl content. Catalyst made oxidized starch had more carbonyl and carboxylgroups, and degraded starch molecules heavily. Meanwhile catalyst accelerated thedecomposition of hydrogen peroxide.
引文
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