高比表面积多孔淀粉制备和改性及在水处理中的应用

采用溶胶-凝胶法成功制备出高比表面积多孔淀粉,并探讨原淀粉种类、悬浮液浓度、聚乙二醇添加剂量和干燥方式等因素对制备出的多孔淀粉比表面积的影响。结果表明,在可溶性淀粉质量分数为15%、聚乙二醇4 g、采用冷冻干燥方式条件下,获得最大比表面积为96 m2/g的多孔淀粉。在多孔淀粉的基础上,制备了多孔淀粉黄原酸酯,并初步考察了其对Pb2+的吸附性能。多孔淀粉进行交联、醚化和胺化改性,制备了多孔胺化淀粉,并简单研究了其对AG25染料分子的吸附情况。     

不同交联处理对玉米多孔淀粉颗粒结构的影响

对玉米淀粉进行醚化交联、酯化交联及醚化、酯化复合交联处理,再酶解为多孔淀粉,考察了不同交联处理方法对多孔淀粉的颗粒形貌、结晶结构、粒度分布、比表面积的影响,与多孔淀粉相比,交联处理后玉米多孔淀粉颗粒仍呈蜂窝状中空结构且晶型保持A型结构,但结晶度分别下降2.22%,1.59%,4.02%;平均粒径分别增加12.34%,10.72%,16.17%,粒径分布的均一度提高;比表面积分别减小15.9%,3.22%,25.89%;平均孔径分别增大7.45%,4.47%,24.25%;比孔容分别增大21.92%,36.46%,67.68%。结果表明,经交联后多孔淀粉的颗粒结构发生了明显变化,为多孔淀粉的进一步开发应用提供了参考。     

机械活化对木薯淀粉的直链淀粉含量及抗性淀粉形成的影响

采用搅拌球磨机对木薯淀粉进行机械活化,研究了机械活化对木薯淀粉中直链淀粉含量的影响,并以抗性淀粉含量作为评价指标,分别考察了活化时间、储存时间、淀粉糊浓度、糊化温度和储存温度对抗性淀粉形成的影响.结果表明,直链淀粉含量随活化时间的延长而增加.适度的机械活化有利于淀粉分子重结晶,抗性淀粉含量显著提高,其它因素对抗性淀粉形成也有较大的影响,且与淀粉的活化时间密切相关.活化时间1 h的样品在制备条件为淀粉糊浓度140 g·L-1、沸水浴糊化20 min、4℃储存36 h时,抗性淀粉含量达到13.81%,而在相同条件下,由原淀粉制备的抗性淀粉含量仅为6.75%.XRD的分析表明,所制备的抗性淀粉属于B型结晶结构.     

多孔淀粉制备工艺优化

在碱法制备大米淀粉的基础上,以大米淀粉为原料,对酶解制备多孔淀粉的工艺条件进行优化。分别考察了酶配比、反应时间、温度、pH、加酶量和底物质量分数6个因素的影响。采用单因素试验法优化了复合酶酶解大米淀粉的工艺条件,并改进了多孔淀粉的分析方法。得到的较佳工艺条件是:温度50℃,时间12 h,pH为4.6,m(α-淀粉酶)∶m(糖化酶)=1∶12,酶质量分数为0.50%,底物质量分数25%。制备的多孔淀粉的吸水率和吸油率分别是125.8%和163.2%,比表面积是2.219m2/g。此工艺可为多孔淀粉工业化生产提供参考数据,并为我国的大米和淀粉资源的综合开发利用提供一条有效途径。     

淀粉接枝丙烯酰胺的制备方法研究

以天然淀粉和丙烯酰胺单体为原料,过硫酸铵为引发剂,合成淀粉接枝丙烯酰胺共聚物(ST-g-PAM)。考察了淀粉种类、聚合方法、油水比、乳化剂配比对接枝效率的影响,对产物结构进行表征。结果表明,以玉米淀粉为原料,淀粉乳糊化20 min,超声处理20 min,水油体积比70∶100,Span80与Tween20质量比7∶1,制备的ST-g-PAM共聚物的单体转化率、接枝率、接枝效率分别为90.56%、38.22%、83.64%,接枝物的结晶度降低。     

玉米淀粉/羧甲基纤维素生物复合凝胶的制备及吸附行为研究

以玉米淀粉与羧甲基纤维素（CMC）为骨架，以丙烯酸（AA）、丙烯酰胺（AM）、2-丙烯酰胺基-2-甲基丙磺酸（AMPS）为单体制备复合凝胶，对复合凝胶材料进行表征。以亚甲基蓝（MB）为吸附质，考察复合凝胶吸附剂对阳离子染料吸附过程的动力学和热力学行为，分析阳离子强度、水体pH值、染料初始质量浓度等对吸附剂吸附性能的影响。结果表明：玉米淀粉-CMC-g-AA-AM-AMPS凝胶是一种表面多孔的吸附材料，其比表面积为24.939 7 m2/g，平均吸附孔径为8.668 2 nm。凝胶对MB的吸附过程与准二级动力学模型和Langmuir模型拟合较好，属于单分子层的化学吸附。阳离子对凝胶吸附MB有明显抑制作用，抑制效果为Al3+>Ca2+>Na+。随着离子强度的增加，抑制作用越明显。在投加量为0.1 g、温度为298 K、pH值为11.0、MB初始质量浓度为2 000 mg/L条件下，吸附剂最大吸附量达到1 938.82 mg/g、去除率为96.94%，能有效去除MB。     

不同直链含量高直链玉米淀粉糊化特性的研究

玻璃纤维是一类具有优异性能的无机非金属材料,在诸多领域都有广泛应用,但在生产过程中需要涂覆浸润剂。淀粉具有较好的成膜性,可以用作玻璃纤维浸润成膜剂,在制备浸润成膜剂时需要对淀粉进行糊化,而且玉米淀粉的质量与其糊化有着直接的关系。通过差示扫描量热法(DSC)可以观察到糊化过程中的相变,在DSC图谱中表现为吸热峰,实验确立测定玉米淀粉糊化适宜条件,在升温速率和水分含量分别为10℃/min和70%下,对国内外五种不同直链含量高直链玉米淀粉进行糊化特性的测定。结果表明:进口淀粉在糊化过程较国内淀粉糊化更平缓,随着直链淀粉含量的增加,糊化峰值温度逐渐增长,热焓变值逐渐减小,说明玉米淀粉直链含量越高,越难以糊化,破坏其结构需要吸收更多能量。     

一种利用玉米淀粉制备胶粘剂的新方法

分析了淀粉胶难以取代泡花碱胶粘剂的原因,选用新型的催化剂,探讨了各种因素对淀粉氧化和糊化的影响及简要机理,得出了制备淀粉胶的最佳条件为：于40％的淀粉乳中加入5％的氧化剂,在催化剂存在时于58℃下氧化30min,加入10％的NaOH糊化,加填料、加水调节固含量至12％(均以淀粉质量为基准),合成的玉米淀粉胶粘剂成本低、干燥快,有望彻底取代泡花碱。将这种胶粘剂进行了工业化试生产,并对应用情况作了简略介绍。     

低成本快干型淀粉胶的研究

选用新型的催化剂,探讨了各种因素对淀粉氧化和糊化的影响,结果表明,制备淀粉胶的最佳条件为:40%的淀粉乳中加入5%的氧化剂,在催化剂存在时于58℃下氧化30min,加入10%的NaOH糊化,加填料、加水调节固含量至12%(均以淀粉质量为基准),合成的玉米淀粉胶粘剂成本低、干燥快,有望彻底取代泡花碱。     

凝胶老化时间对炭气凝胶结构及电化学性能影响

以间苯二酚、间苯三酚、甲醛为反应原料,碳酸钠为催化剂,羧化壳聚糖作为软模板,通过溶胶-凝胶、丙酮置换、常压干燥和高温热解制备炭气凝胶。利用红外光谱(IR)、比表面积及孔径分析(BET)、扫描电镜(SEM)和电化学分析手段,对比讨论了不同凝胶老化时间对炭气凝胶的结构和电化学性能的影响。实验结果表明,随着凝胶老化时间的延长,炭气凝胶的平均孔径逐渐增大,比表面积逐渐减小,总孔体积逐渐增大,比电容逐渐减小。凝胶老化时间为12 h时生成的炭气凝胶,具有最大的比表面积(659.17 m2/g),比电容也达到最大值,在1.0 A/g电流密度下比电容为144.38 F/g。     

Fabrication of 3D-networks of native starch and their application to produce porous inorganic oxide networks through a supercritical route

Herein an effective method for fabrication of three dimensional networks of starch is presented. In this method, the native starch was dissolved in hot water to form solution, resulting in the formation of starch gel after cooled to room temperature. Then the water in the starch gel was exchanged by ethanol, followed by drying with supercritical (SC) CO₂ extraction, the nano-networks of starch were prepared. The obtained starch aerogel was composed of starch fibers and presented porous structure. Changing the initial concentration of native starch and controlling the drying conditions could control the microstructure of the starch networks. The resulting starch networks were utilized as a directing template to prepare the hierarchically ordered TiO₂ networks. In this process, TiO₂ precursor dissolved in SC CO₂ diffused onto the surface of starch gel, and reacted with the hydroxyl groups and adsorbed water molecules on the starch surface, to form an organic/inorganic hybrid material. After calcining the composites at 500 °C, the networks composed of anatase TiO₂ nanocrystals were produced, which accurately replicated the fine structures of the starch gel and possessed higher BET surface area and total pore volume compared with those of other TiO₂ materials templated by some biomaterials or polymer gels.     

淀粉基多孔碳材料的制备及其吸附CO2/CH4性能

以淀粉为原料,使用水热法将其碳化后用活化剂KOH对其活化,制备了淀粉基多孔碳材料,并对其进行结构表征和CO₂/CH₄的吸附性能测试,计算吸附热以及材料对CO₂/CH₄的吸附选择性,讨论了碳材料结构对其吸附性能的影响。结果表明：在制备过程中,随着活化剂KOH用量比例的增大,所制得的材料其比表面积和孔容增大,其孔径分布也就越宽。所制得的碳材料其比表面积可达2972 m²·g^-1。这些淀粉基多孔碳材料对水蒸气的吸附等温线呈现出Ⅳ类等温线。所制备材料对CO₂吸附容量主要取决于其孔径小于0.8 nm的累积孔容（Vd < 0.8 nm）。材料的超微孔的孔容越大,其对CO₂吸附容量也越大。所制备的C-KOH-1材料在101325 Pa和298 K条件下,对CO₂的吸附量达到4.2 mmol·g^-1,其对CO₂的吸附热明显高于其对CH₄吸附热,其对CO₂/CH₄吸附选择性为3.7～4.26,同时本文通过对材料的水蒸气吸附等温线进行测试,结果表明所得材料主要表现为中等憎水性,这对材料在实际工况的应用奠定了基础。     

正交法优化淀粉接枝共聚高吸水树脂的工艺条件

以过硫酸钾为引发剂,甘油溶液为交联剂,引发甘薯淀粉与丙烯酸接枝共聚反应。对影响反应的主要因素如丙烯酸中和度、引发剂的量、交联剂的量、体系用水量、淀粉糊化时间进行了研究。结果表明,淀粉接枝丙烯酸共聚高吸水树脂的最佳工艺条件为:丙烯酸中和度为70%,引发剂的量为60 mg,交联剂量为0.25 mL,体系用水量为40 mL,淀粉糊化时间为20 min。按此条件制得的树脂的吸水率为768 g/g     

Preparation of homogeneous mullite‐based fibrous ceramics by starch consolidation

Silica sol is one of the frequently used binders in high‐temperature resisting fibrous porous ceramics, but in the drying process, it can diffuse with water and influence the uniformity of ceramics. To solve this diffusion problem and fabricate homogeneous fibrous porous ceramics, cationic starch was firstly introduced in mullite fibrous system. The effects of starch content and high‐temperature binder content on microstructure, physical, and mechanical properties were also investigated. The results indicate that starch consolidated mullite fibrous ceramics owned a homogeneous 3D skeleton structure, since the introduced starch can absorb both water and silica particles by gelatinization and ensure the even distribution of binders. Compared with the mullite fibrous ceramics fabricated without starch addition, starch consolidated ceramics owned better microstructure and higher interior compression strength. Furthermore, both the starch and silica sol content had great impact on the microstructure, density, porosity, thermal conductivity, and compressive strength of the fibrous ceramic.     

制备工艺对淀粉基碳分子筛性能的影响

以淀粉为碳源,F127为结构导向剂,通过KOH活化一步合成法制备系列碳分子筛,采用SEM、TG、FT-IR和N_2吸附-脱附等技术对原料和碳分子筛样品的结构、表面官能团和性能进行表征。结果表明,温度、F127与淀粉添加质量比和KOH浓度对碳分子筛样品的孔隙结构性能影响显著。在KOH浓度为0.75 mol·L~(-1)、m(F127)∶m(淀粉)=4∶3、搅拌时间12 h和反应温度45℃时制备的碳分子筛孔径分布集中,BET比表面积达1 228.972 5 m~2·g~(-1),单点孔容0.807 113 cm~3·g~(-1),单点微孔体积0.636 869 cm~3·g~(-1)。     

Investigation on the adsorption behaviour of heating-treated starch on hematite

An investigation on these adsorption characteristics of heating-treated starch on fine hematite was conducted through a series of tests, like adsorption tests, zeta potential tests, micro-flotation tests and Fourier transform infrared spectroscopic analysis as well. All results pointed out that different temperature of starch heating treatment tends to achieve different degree of starch gelatinization, probably contributing to its different flocculating capacities on mineral surfaces. Since such differences on the degree of starch gelatinization after heating-treatment seem to induce distinct amounts of adsorption densities and flocculated recoveries on hematite. And the higher the water temperature is, the better the starch gel would be.     

Pore size control of porous silica by sol-gel process

Porous silica glass was prepared by sol-gel process from tetraethoxysilane (TEOS). The effects of solvents (water, ethanol), drying condition, heat treatment temperature on specific surface area and pore size distribution of porous silica were investigated. Gelation process accelerates with an increase of H₂O content, while retards with the increase of ethanol amount. Structure changes during heat treatment were studied by means of DTA, XRD. TEM micrographs show that the gel particles shrink after heated at 500°C, thus the average pore size decreases.     

Preparation and characterization of porous alumina ceramics through starch consolidation casting technique

This work aims at studying the influence of thermal treatment on the microstructure, resistivity and technological properties of porous alumina ceramics prepared via starch consolidation casting (SCC) technique. Colloidal suspensions were prepared with three different contents of alumina solid loading (55, 60 and 65 mass%) and corn starch (3, 8 and 13 mass%). The sintered samples at 1400, 1500, 1600 and 1700 °C, show open porosity between 46 and 64%, depending on the starch content in the precursor suspensions and sintering temperature. The pore structures were analyzed by SEM. The effect of corn starch content on the apparent porosity, pore size distribution, linear shrinkage and electrical resistivity as well as cold crushing strength of the sintered porous alumina ceramics was also measured. These porous alumina ceramics are promising porous ceramic materials for using in a wide range of thermal, electrical and bioceramics applications as well as filters/membranes and gas burners, due to their excellent combination properties.     

Preparation and properties of biodegradable thermoplastic starch/poly(hydroxy butyrate) blends

The vital differences using three types of thermoplastic starches (TPS), including potato starch, corn starch, and soluble potato starch, with two different gelatinization degrees to blend with poly(hydroxy butyrate) (PHB) are thoroughly discussed in this study. For blends containing a certain amount of PHB, thermal stability remains in a certain degree. In all cases of this study, mechanical properties of TPS blended with PHB confer higher performance than those of pristine TPS. In particular, a significant increase on tensile strength and tear strength is observed for TPS (potato starch) blended with PHB at low gelatinization degree. A suitable degree of gelatinization of starch is critical to achieve optimum performance. The investigation on the morphological observation partly features the supporting evidence of the above findings. The assessment of biodegradability indicates that the values of water absorption and weight loss increase with increasing treatment period and glycerol content, but decrease with increasing amount of PHB content. Among three types of starches investigated, the TPS (soluble starch)/PHB blend gives the highest level of water absorption and weight loss. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 2371–2379, 2006