机械活化干法制备硬脂酸木薯淀粉酯

为获得制备硬脂酸淀粉酯的新工艺,采用机械活化干法制备木薯硬脂酸淀粉酯。以取代度和反应效率为指标,分别探讨硬脂酸用量、盐酸用量、球磨温度、球磨时间、搅拌速度、球磨介质的堆体积等因素对木薯淀粉硬脂酸酯反应的影响,并对影响因素进行了正交优化。结果表明,机械活化明显提高了木薯淀粉的酯化反应活性。通过正交试验确定了制备硬脂酸酯的最佳工艺条件为:硬脂酸质量分数5%、盐酸质量分数0.14%、球磨温度50℃、球磨时间60 min、搅拌速度380 r/min、球磨介质堆体积500 mL,在此条件下制备的木薯硬脂酸酯淀粉的取代度为0.007 1,反应效率为28.77%。并采用红外光谱(FTIR)、X-射线衍射(XRD)、扫描电镜(SEM)对木薯硬脂酸淀粉酯的结构进行了表征。检测结果显示,木薯硬脂酸淀粉酯具有良好的乳化能力。     

机械活化木薯淀粉制备低取代度醋酸酯淀粉的研究

以机械活化0.5h的木薯淀粉和木薯原淀粉为原料,以醋酸酐为酯化试剂,氢氧化钠为催化剂,制备低取代度木薯淀粉醋酸酯。以淀粉醋酸酯的取代度和反应效率为评价指标,分别研究反应温度、反应时间、醋酸酐用量、pH各因素对其取代度和反应效率的影响。实验结果表明,反应温度、反应时间、醋酸酐用量、pH对木薯淀粉醋酸酯的取代度和反应效率均有影响。机械活化能显著提高木薯淀粉醋酸酯化反应的取代度和反应效率。通过试验得到制备低取代度木薯淀粉醋酸酯的较佳工艺条件为:反应温度为30℃,反应时间为40min,醋酸酐用量为0.15mL,pH为8.5时,在此条件下制备的醋酸酯淀粉的取代度为0.075、反应效率为87.45%。并用红外光谱对醋酸酯淀粉进行分析。     

活化处理方法对制备柠檬酸淀粉酯的影响

采用三种不同方式预先对淀粉进行活化,然后以活化淀粉为原料,以柠檬酸为酯化剂制备柠檬酸淀粉酯。探讨了活化方式、原料配比、催化剂用量、反应温度及反应时间对淀粉酯化取代度的影响。对淀粉柠檬酸酯的糊化透明度及乳化效果进行测试。结果表明,胰酶活化对淀粉酯化效果影响较显著。柠檬酸淀粉酯的最佳合成条件是:淀粉柠檬酸质量比2∶1,催化剂为淀粉质量的3%,反应时间5h,反应温度70℃时,制备的淀粉酯取代度为0.412。随着淀粉酯取代度增大,淀粉糊透明度升高,乳液稳定性先升高后稍有回落。     

微波-超声波辅助制备羟丙基木薯淀粉及表征

以木薯淀粉为原材料,环氧丙烷为醚化剂,氢氧化钠为催化剂,在微波-超声波辅助条件下制备羟丙基木薯性淀粉。采用紫外可见分光光度计测量羟丙基木薯淀粉取代度,研究了微波功率、超声波功率、反应时间、环氧丙烷用量、淀粉质量浓度、氢氧化钠用量对羟丙基木薯淀粉取代度的影响。通过单因素实验及正交实验获得制备羟丙基木薯淀粉的最佳实验条件,并采用X射线衍射分析(XRD)、场发射扫描电镜(FESEM)对其进行表征。结果表明:最佳制备羟丙基木薯淀粉条件为淀粉质量浓度为20%,环氧丙烷用量为2 m L,反应时间为2.5 min,微波:超声波功率为24W:500 W,氢氧化钠用量为淀粉质量的0.7%;X射线衍射,场发射扫描电镜表明羟丙基木薯淀粉的形态发生部分变化,反应主要发生在无定型区。     

机械活化固相化学反应制备木薯醋酸酯淀粉

为获得制备醋酸酯淀粉的新工艺,采用机械活化固相化学反应法制备木薯醋酸酯淀粉。以醋酸酯淀粉的取代度为评价指标,分别探讨醋酸酐用量、NaOH用量、球磨温度、球磨时间、搅拌速度、球磨介质的堆体积等因素对木薯淀粉醋酸酯反应的影响,并对影响因素进行了正交优化。结果表明:在醋酸酐质量分数60%、NaOH质量分数2.0%、球磨温度60℃、球磨时间60 min、搅拌速度380 r/min、球磨介质堆体积500 mL的反应条件下,制备得到的木薯醋酸酯淀粉的取代度为0.263 2,反应效率为25.57%。并采用红外光谱(FTIR)、X-射线衍射(XRD)对木薯醋酸酯淀粉的结构进行了表征。机械活化对淀粉发生酯反应有显著的强化作用。     

微波法制备硬脂酸木薯淀粉酯

目的建立微波辅助技术制备硬脂酸木薯淀粉酯,并对其理化性质进行表征。方法以木薯淀粉为原料,以硬脂酸为酯化剂,以盐酸为催化剂,通过均匀设计实验并经SPSS 10.0软件优化微波法制备硬脂酸木薯淀粉酯的最佳工艺参数。结果硬脂酸木薯淀粉酯的最佳工艺条件如下:淀粉50 g(干基),微波功率450 W,微波辐射时间1.5 min,盐酸加入量6.0 mL,硬脂酸0.5 g,得到的产品取代度为0.01685。结论本研究建立了一种无污染、反应快、能耗低的硬脂酸木薯淀粉酯制备方法,得到的产品取代度较高,溶解度、乳化性和乳化稳定性均优于原淀粉。     

微波辐射合成醋酸酯淀粉的研究

本文以玉米淀粉为原料,以醋酸酐为乙酰化试剂,氢氧化钠为催化剂,利用微波辐射技术对醋酸酯淀粉的合成工艺进行了研究.探讨了醋酸酐用量、淀粉含水量、微波辐射时间、微波辐射功率、氢氧化钠浓度等因素对醋酸酯淀粉乙酰基含量的影响.通过正交试验得到了微波辐射合成醋酸酯淀粉的最佳工艺为:醋酸酐用量80%,加水量2g,辐射时间5min,辐射功率200W,取代度为0.138 6.并对产物的结构与性能进行了测定.     

木薯淀粉交联羧甲基化改性及工艺优化

用搅拌球磨机活化木薯淀粉,将经活化60 min的木薯淀粉用环氧氯丙烷进行适度交联,再将交联淀粉与一氯乙酸钠通过干法工艺制备交联羧甲基复合淀粉.以取代度为评价指标,探讨交联度、反应温度、反应时间、一氯乙酸钠用量、氢氧化钠用量和含水量等因素对淀粉羧甲基化反应的影响,通过正交试验优化制备条件.结果表明,使用中等交联度的交联淀粉在反应时间150 min、反应温度55℃、淀粉与一氯乙酸钠的摩尔比0.55、淀粉与氢氧化钠的摩尔比0.50,体系含水量24％的条件下制得的复合淀粉取代度为0.841.     

机械活化木薯淀粉干法制备氧化淀粉的研究

采用搅拌球磨机对木薯淀粉进行机械活化,以不同活化时间的木薯淀粉为原料、CuSO4为催化剂、H2O2为氧化剂干法制备氧化淀粉,并以羧基含量为评价指标,分别考察了活化时间、反应时间、反应温度、氧化剂用量、催化剂用量、pH值、体系含水量等因素对木薯淀粉氧化反应的影响.实验结果表明,机械活化对木薯淀粉的氧化反应有显著的强化作用,活化时间越长,木薯淀粉被氧化的程度越深,羧基含量越高.活化1 h的样品在制备条件为反应时间120 min、H2O2与淀粉的摩尔比0.586、催化剂CuSO4在淀粉中的质量分数0.03%、反应温度50℃、体系含水量27.37%、体系pH值等于5时制得的氧化淀粉羧基含量为0.81%,而在相同条件下,由原木薯淀粉制得的氧化淀粉羧基含量仅为0.26%.     

机械活化辛烯基琥珀酸西米淀粉酯的制备及其乳化性能分析

采用自制搅拌式球磨机对西米淀粉进行机械活化预处理,以辛烯基琥珀酸酐为酯化剂制备辛烯基琥珀酸西米淀粉酯。探讨活化时间、反应时间、辛烯基琥珀酸酐添加量、反应温度和pH等因素对辛烯基琥珀酸西米淀粉酯取代度的影响。结果表明,机械活化对西米淀粉辛烯基琥珀酸酐酯化反应有明显的增强作用;在相同反应条件下,活化淀粉的取代度和反应效率显著上升;通过正交试验确定了活化1.0 h西米淀粉酯的最佳工艺条件：反应时间为2.0 h,辛烯基琥珀酸酐用量为3%,pH为8.0,反应温度为35℃;在此条件下酯化得到的淀粉酯取代度为0.02294,反应效率为98.01%。FTIR、XRD、SEM测试结果表明,西米淀粉经过辛烯基琥珀酸酐处理后,产品的红外光谱在1570 cm^-1和1712 cm^-1处出现了新的吸收峰,淀粉结晶度下降,淀粉颗粒表面受到破坏,颗粒中间出现较大孔洞,进一步证实西米淀粉发生了酯化反应。取代度为0.02294的辛烯基琥珀酸西米淀粉酯的乳化性为26.43%,乳化稳定性为24.10%,均优于原西米淀粉酯。     

The Role of Reaction Parameters on the Preparation and Properties of Carboxymethyl Cassava Starch

The role of reaction variables on carboxymethylation of cassava starch was investigated using a statistically experimental design approach. The reaction was carried out in an isopropanol‐water mixture at 40°C for 3 h. The reaction parameters under investigation included water fraction in the reaction medium, the ratio of sodium hydroxide to anhydroglucose unit (AGU) and the ratio of sodium monochloroacetate (SMCA) to AGU. The dependent responses were degree of substitution (DS) of CMS and the reaction efficiency (RE) of the carboxymethylation. Carboxymethyl cassava starches with DS in the range of 0.01 to 0.86 were prepared. The result from regression analysis indicated that the most important factors in controlling the DS of CMS were sodium hydroxide and SMCA contents followed by water content. Response surface plots suggested that the optimal levels of sodium hydroxide and water content to achieve CMS with high DS were at the intermediate values. Similar effects of sodium hydroxide and water content were also observed on the RE while SMCA content had a negative effect; increasing SMCA content resulted in lower RE. The optimal conditions to achieve the highest DS and RE were found to be at a water content of 17–19% with a molar ratio of sodium hydroxide to AGU of 1.8–1.9 and a molar ratio of SMCA to AGU between 1.1–1.5. Carboxymethyl cassava starch with various DS was also prepared. The properties of CMS as affected by the degree of modification were also discussed.     

乙酰化柠檬酸酯化交联机械活化淀粉的制备及性质分析

以机械活化木薯淀粉为原料,醋酸酐为酯化剂,柠檬酸为交联剂,采用溶剂法制备乙酰化柠檬酸酯化交联淀粉,考察了机械活化时间、混合酸添加量、反应温度、反应时间、柠檬酸与乙酸酐质量比等因素对乙酰化柠檬酸酯化交联淀粉沉降积的影响,并对制备得到的酯化交联淀粉进行结构表征及性质测定.结果表明,制备最佳工艺条件为:机械活化时间40 mi...     

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

以木薯淀粉为原料,氯乙酸钠为醚化剂,氢氧化钠为催化剂,采用机械活化固相化学反应法制备羧甲基淀粉。以取代度为评价指标,通过单因素和正交试验设计优化确定最佳制备工艺,采用傅里叶红外光谱（Fourier transform infrared spectroscopy,FTIR）、X-射线衍射（x-ray diffraction,XRD）、扫描电镜（scanning electron microscope,SEM）对羧甲基淀粉的结构进行表征,并考察羧甲基淀粉的理化特性。结果表明,最佳工艺参数为淀粉与氯乙酸钠物质的量比1∶1、反应温度50?℃、反应时间1.5?h、氢氧化钠溶液质量分数18.8%、搅拌速率380?r/min、球磨介质堆体积500?mL,在此条件下制备的羧甲基淀粉取代度为0.540?1。FTIR、XRD、SEM检测进一步证实木薯淀粉发生了羧甲基化反应。理化特性结果显示,羧甲基淀粉的黏度升高,溶解度增大,吸水性、保水性、冻融稳定性、抗酸碱性、抗酶解性等均得到较好的提高。     

Studies on the properties of citrate derivatives of cassava (Manihot esculenta Crantz) starch synthesized by microwave technique

Cassava starch citrates with degree of substitution (DS) ranging from 0.005 to 0.063 were synthesized by the microwave‐assisted reaction of cassava starch with citric acid. A response surface small composite design was used to study the effect of different reaction conditions, viz. time, temperature and reagent concentration. All these variables significantly affected the substitution level in the modified starches. The DS increased with increase in the time of reaction and temperature. However, reagent concentration had a negative effect on the DS. The modified starches showed higher viscosity with lower breakdown, lower setback and higher final viscosities in comparison to native starch. Differential scanning calorimetry showed that the modified starches exhibited a decrease in gelatinization temperatures, T_o, T_p, T_e, in comparison to native starch. However, the heat of gelatinization was not significantly affected. The citrate derivatives exhibited reduced swelling volume and enhanced water binding capacities. They were found to be less susceptible to enzyme hydrolysis than native starch. Copyright © 2007 Society of Chemical Industry     

Synthesis of Octenyl Succinic Derivative of Mechanically Activated Indica Rice Starch

Indica rice starch was mechanically activated by ball milling and then esterified by octenyl succinic anhydride (OSA) in aqueous slurry systems. The process of esterification was studied with respect to the time of mechanical activation, OSA/starch ratio, temperature, pH, starch slurry concentration and reaction time. The effects of these reaction conditions were evaluated on the basis of degree of substitution (DS) and reaction efficiency (RE). The results indicated that mechanical activation could enhance the reaction of OSA and starch. The DS and RE of OSA starch increased sharply when the time of mechanical activation increased from 0 h to 10 h, after which it was not significantly affected until 50h. The suitable conditions for the synthesis of OSA starch from Indica rice starch that was mechanically activated for 10 h (MAIS10) were an OSA/starch ratio 3%, temperature 35°C, pH 8.5, starch slurry concentration 12.5% and reaction time 3h. For native Indica rice starch (NIS), all conditions were identical to MAIS10 except for the starch slurry concentration of 40% and reaction time of 4 h. The maximum DS and RE of OSA‐MAIS10 (0.02037, 88.03%) was higher than that of OSA‐NIS (0.01700, 73.46%) at OSA/starch ratio 3%. The esterification of MAIS10 with OSA showed a low sensitivity to pH and a higher stability than OSA‐NIS. Scanning electron microscopy (SEM) revealed that the modified OSA starches did not show any detectable change in the morphological structural characteristics. The esterification between OSA and starch was confirmed by Fourier transform infrared (FT‐IR) spectroscopy.     

微波辅助干法制备阳离子木薯淀粉

采用微波辅助加热法干法制备阳离子淀粉,详细考察了微波功率、微波辐照时间、氢氧化钠用量和3-氯-2-羟丙基三甲基氯化铵醚化剂(CHPTMA)用量等对反应效率及其产品取代度的影响。结果表明:微波干法合成阳离子淀粉,反应时间短,反应效率高;在NaOH分2次加入、NaOH与淀粉质量比为4.0%、醚化剂用量为淀粉质量的4.5%、水用量为淀粉用量的25.0%、微波功率为450 W及微波辐照时间为3.0 min等条件下,阳离子淀粉取代度为0.037 5,阳离子醚化剂反应效率高达93.76%。     

高取代度羧甲基小麦淀粉制备工艺的优化及表征

摘 要：以小麦淀粉为原料,以氯乙酸作为醚化剂,采用两次加碱法制备了高取代度的羧甲基小麦淀粉。以4.05g淀粉为基准,采用正交实验对反应条件进行了优化,得到的最佳工艺条件为：水用量6mL,无水乙醇用量60mL,氯乙酸与淀粉摩尔比1.4,氢氧化钠与氯乙酸摩尔比1.8,碱化用氢氧化钠百分比70%,碱化温度35～40℃,碱化时间0.5～1h,醚化温度50～55℃,醚化时间2～3h,在此条件下制得了取代度高达1.21的羧甲基小麦淀粉。     

Development and Physicochemical Characterization of New Resistant Citrate Starch from Different Corn Starches

Resistant starch has drawn broad interest for both potential health benefits and functional properties. In this study, a technology was developed to increase resistant starch content of corn starch using esterification with citric acid at elevated temperature. Waxy corn, normal corn and high‐amylose corn starches were used as model starches. Citric acid (40% of starch dry weight) was reacted with corn starch at different temperatures (120–150°C) for different reaction times (3–9 h). The effect of reaction conditions on resistant starch content in the citrate corn starch was investigated. When conducting the reaction at 140°C for 7 h, the highest resistant starch content was found in waxy corn citrate starch (87.5%) with the highest degree of substitution (DS, 0.16) of all starches. High‐amylose corn starch had 86.4% resistant starch content and 0.14 DS, and normal corn starch had 78.8% resistant starch and 0.12 DS. The physicochemical properties of these citrate starches were characterized using various analytical techniques. In the presence of excess water upon heating, citrate starch made from waxy corn starch had no peak in the DSC thermogram, and small peaks were found for normal corn starch (0.4 J/g) and Hylon VII starch (3.0 J/g) in the thermograms. This indicates that citrate substitution changes granule properties. There are no retrogradation peaks in the thermograms when starch was reheated after 2 weeks storage at 5°C. All the citrate starches showed no peaks in RVA pasting curves, indicating citrate substitution changes the pasting properties of corn starch as well. Moreover, citrate starch from waxy corn is more thermally stable than the other citrate starches.     

半干法制备高取代度阳离子淀粉及表征

以玉米淀粉为原料,利用N-(2,3- 环氧丙基)三甲基氧化铵(GTA)为醚化剂,在NaOH 为催化剂条件下,通过半干法制备阳离子淀粉。实验表明：对阳离子淀粉取代度(DS)影响的因素顺序依次为：反应时间＞反应温度＞体系中含水量＞氢氧化钠用量。当淀粉用量为10g、GTA 用量为1.5g、NaOH 0.2g、反应温度80℃、反应时间4h、体系中含水量24% 时,DS 可达到0.105。对不同取代度的阳离子淀粉进行理化性质分析及表征,结果表明：阳离子淀粉的透明度、溶解度均随着取代度的增高有所增加。通过对阳离子淀粉进行红外光谱、偏光分析和X 射线衍射分析,证实取代反应过程中淀粉结构发生了一定程度的变化。