微孔淀粉、交联微孔淀粉以及交联微孔淀粉微球的制备及其应用研究
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摘要
本学位论文以微孔淀粉、交联微孔淀粉以及交联微孔淀粉微球的制备、性能测定及其应用研究为课题,以玉米淀粉为原料,分别通过对原淀粉进行酶解反应制得微孔淀粉,对微孔淀粉进行交联反应制得交联微孔淀粉,以及对微孔淀粉通过反相乳液聚合法进行两次交联制得交联微孔淀粉微球。同时,对反应后的产物的吸附性能进行了测定,并对反应过程中所有可能影响产物吸附率的因素进行了系统的考察,优化了反应条件。另外,对微孔淀粉制备过程中,酶解反应时的水解率、交联微孔淀粉制备过程中产物的交联度、冻融稳定性等进行了研究。最后,考察了交联微孔淀粉微球对尼古丁的吸附性能。具体包括以下五个方面内容：
1.采用酶解反应制备了微孔淀粉。在酶解反应过程中,分别对α-淀粉酶与糖化酶的质量比(mα-淀粉酶／m糖化酶)、酶的总质量与淀粉的质量之比(m总酶／m淀粉)、溶液的总体积与淀粉的质量之比(V溶液／m淀粉)、体系的pH值、酶解反应的温度以及反应时间对产物色素吸附率的影响进行了系统的考察,根据以上结果确定出了该方法制备微孔淀粉的最佳反应条件；对各个反应条件下的水解率进行了考察,并对其结果与色素吸附率的结果进行了对比；通过傅立叶变换红外光谱对比了原淀粉与微孔淀粉结构的异同,用扫描电子显微镜观察了玉米原淀粉微孔化前后表面形貌的变化,利用X-射线粉末衍射表征了微孔淀粉结晶度的变化,用示差扫描量热仪考察了微孔淀粉糊化温度的变化。
2.以上述制得的微孔淀粉为原料,通过交联反应制备了交联微孔淀粉。探讨了碱化过程中的氯化钠与淀粉的质量比(mNacl／m淀粉)、氢氧化钠与淀粉的质量比(mNaOH／m淀粉)、碱化温度、碱化时间,以及交联过程中的交联剂环氧氯丙烷的体积与淀粉的质量比(V环氧氯丙烷／m淀粉)、溶液的总体积与淀粉的质量比(V溶液／m淀粉)、体系pH值、交联反应温度、交联反应时间等因素对产物色素吸附率的影响,得出了该方法制备交联微孔淀粉的最佳反应条件；通过傅立叶变换红外光谱对比了原淀粉与交联微孔淀粉结构的异同,使用扫描电子显微镜观察了交联微孔淀粉的表面形貌。
3.对以上制得的交联微孔淀粉的性能进行了研究。考察了各个反应条件与产物的交联度以及产物的冻融稳定性之间的关系；用X-射线粉末衍射表征了交联微孔淀粉结晶度的变化,用示差扫描量热仪考察了交联微孔淀粉糊化温度的变化。
4.以上述制得的微孔淀粉为原料,通过反相乳液聚合法对其进行两次交联反应,制得了交联微孔淀粉微球。考察了在第一次交联过程中不同乳化剂(司班60、司班80、吐温60、吐温80)、环己烷与水的体积比(V环己烷／V水)、乳化剂司班60与吐温80的质量之比(m司班6dm吐温80)、乳化剂的总质量与环己烷的体积之比(m乳化剂总量／V环己烷)、淀粉的质量与水的体积之比(m淀粉/V水)、交联剂N,N’-亚甲基双丙烯酰胺与淀粉的质量比(mNNMBA／m淀粉)、引发剂硝酸铈铵与淀粉的质量比(mCAN／m淀粉)、交联反应温度和交联反应时间,以及第二次交联过程中交联剂环氧氯丙烷的体积与淀粉的质量比(V环氧氯丙烷／m淀粉)、交联反应温度和交联反应时间对产物色素吸附率的影响,并根据以上结果确定出了该方法制备交联微孔淀粉微球的最佳反应条件；通过傅立叶变换红外光谱对比了交联微孔淀粉微球与原淀粉的结构差异,用扫描电子显微镜观察了其表面形貌,利用X-射线粉末衍射表征了其结晶度的变化,用示差扫描量热仪考察了其糊化温度的变化。
5.考察了以上制得的交联微孔淀粉微球对尼古丁的吸附性能。
In this thesis, the preparation, performance determination and application of microporous starch, crosslinked microporous starch and crosslinked microporous starch microspheres was carried out. The microporous starch was obtained by enzymatic hydrolysis with native corn starch, and the crosslinked microporous starch was prepared by crosslinking with the microporous starch, and the crosslinked microporous starch microspheres was synthesized in final by two-steps crosslinking with the microporous starch via the method of inverse emulsion polymerization. After that, the adsorption properties of products were mearsured. The factors which can affect the adsorption rate of products were investigated in systematically. According to the results, the reaction conditions were optimized. Besides, the hydrolysis rate was studied in the microporous starch synthesizing process. After the products of crosslinked microporous starch prepared, the crosslinking degree and freeze-thaw stability of them were investigated. Finally, the adsorption properties of crosslinked microporous starch microspheres were studied with nicotine. The main results were summarized as follows:
1. The microporous starch was obtained by enzymatic hydrolysis reaction. During the process, the main reaction conditions which are expected to affect adsorption rate of the products were investigated systematically, including mα-amylase/mglucoamylase, menzyme/mstarch, Vsolution/mstarch, pH, temperature and time of enzymatic reaction. According to the results, the optimal reaction conditions were obtained. Moreover, the hydrolysis rates in each reaction conditions were studied to realize the relationship between the hydrolysis rates and adsorption rates. FTIR was used to compare the structural differences between the native corn starch and microporous starch. SEM images displayed the morphology changes after the treatment with enzyme. The results of XRD showed the changes in crystallinity. DSC determined that the variation of gelatinization temperature.
2. The crosslinked microporous starch was prepared by crosslinking with the microporous starch, which obtained by last step. The effect of each reaction condition on adsorption rate of the products is studied systematically, which included NaOH/mstarch, reaction temperature and time of alkalization, VECH/mstarch, h, pH, reaction temperature and time of crosslinking. The optimal reaction conditions were obtained. FTIR spectra showed the characteristic peaks of the crosslinked microporous starch. And SEM photos revealed its surface morphology.
3. The performance of crosslinked microporous starch prepared by last step was investigated. The relationships among each reaction condition, crosslinking degree of the products, and freeze-thaw stability were studied, In order to study that the changes in crystallinity, the native corn starch and crosslinked microporous starch were examined by XRD. DSC traces showed the alteration in gelatinization temperature.
4. The crosslinked microporous starch microspheres was synthesized by two-steps crosslinking with the microporous starch via the method of inverse emulsion polymerization. The influence of reaction conditions to adsorption rate of the products, such as the different emulsifier (span 60, span 80, tween 60, tween 80), Vcyclohexane/Vsolution, mspan 60/mtween 80?,memulsifie/Vcyclohexane, mstarch/Vsolution, mNNMBA/mstarch, mCAN/mstarch, temperature and time of the crosslinking reaction with NNMBA, h, temperature and time of the crosslinking reaction with ECH, were investigated. The optimal reaction conditions about this method were obtained. Besides, the samples were characterized by FTIR, SEM, XRD and DSC.
5. The experiments for absorbing nicotine of crosslinked microporous starch microspheres were conducted. According to the results, the adsorption kinetics and thermodynamics in this process were investigated. polymerization; adsorption rate; hydrolysis rate; settlement volume; adsorption nicotine; adsorption kinetics; adsorption thermodynamics
1.采用酶解反应制备了微孔淀粉。在酶解反应过程中,分别对α-淀粉酶与糖化酶的质量比(mα-淀粉酶／m糖化酶)、酶的总质量与淀粉的质量之比(m总酶／m淀粉)、溶液的总体积与淀粉的质量之比(V溶液／m淀粉)、体系的pH值、酶解反应的温度以及反应时间对产物色素吸附率的影响进行了系统的考察,根据以上结果确定出了该方法制备微孔淀粉的最佳反应条件；对各个反应条件下的水解率进行了考察,并对其结果与色素吸附率的结果进行了对比；通过傅立叶变换红外光谱对比了原淀粉与微孔淀粉结构的异同,用扫描电子显微镜观察了玉米原淀粉微孔化前后表面形貌的变化,利用X-射线粉末衍射表征了微孔淀粉结晶度的变化,用示差扫描量热仪考察了微孔淀粉糊化温度的变化。
2.以上述制得的微孔淀粉为原料,通过交联反应制备了交联微孔淀粉。探讨了碱化过程中的氯化钠与淀粉的质量比(mNacl／m淀粉)、氢氧化钠与淀粉的质量比(mNaOH／m淀粉)、碱化温度、碱化时间,以及交联过程中的交联剂环氧氯丙烷的体积与淀粉的质量比(V环氧氯丙烷／m淀粉)、溶液的总体积与淀粉的质量比(V溶液／m淀粉)、体系pH值、交联反应温度、交联反应时间等因素对产物色素吸附率的影响,得出了该方法制备交联微孔淀粉的最佳反应条件；通过傅立叶变换红外光谱对比了原淀粉与交联微孔淀粉结构的异同,使用扫描电子显微镜观察了交联微孔淀粉的表面形貌。
3.对以上制得的交联微孔淀粉的性能进行了研究。考察了各个反应条件与产物的交联度以及产物的冻融稳定性之间的关系；用X-射线粉末衍射表征了交联微孔淀粉结晶度的变化,用示差扫描量热仪考察了交联微孔淀粉糊化温度的变化。
4.以上述制得的微孔淀粉为原料,通过反相乳液聚合法对其进行两次交联反应,制得了交联微孔淀粉微球。考察了在第一次交联过程中不同乳化剂(司班60、司班80、吐温60、吐温80)、环己烷与水的体积比(V环己烷／V水)、乳化剂司班60与吐温80的质量之比(m司班6dm吐温80)、乳化剂的总质量与环己烷的体积之比(m乳化剂总量／V环己烷)、淀粉的质量与水的体积之比(m淀粉/V水)、交联剂N,N’-亚甲基双丙烯酰胺与淀粉的质量比(mNNMBA／m淀粉)、引发剂硝酸铈铵与淀粉的质量比(mCAN／m淀粉)、交联反应温度和交联反应时间,以及第二次交联过程中交联剂环氧氯丙烷的体积与淀粉的质量比(V环氧氯丙烷／m淀粉)、交联反应温度和交联反应时间对产物色素吸附率的影响,并根据以上结果确定出了该方法制备交联微孔淀粉微球的最佳反应条件；通过傅立叶变换红外光谱对比了交联微孔淀粉微球与原淀粉的结构差异,用扫描电子显微镜观察了其表面形貌,利用X-射线粉末衍射表征了其结晶度的变化,用示差扫描量热仪考察了其糊化温度的变化。
5.考察了以上制得的交联微孔淀粉微球对尼古丁的吸附性能。
In this thesis, the preparation, performance determination and application of microporous starch, crosslinked microporous starch and crosslinked microporous starch microspheres was carried out. The microporous starch was obtained by enzymatic hydrolysis with native corn starch, and the crosslinked microporous starch was prepared by crosslinking with the microporous starch, and the crosslinked microporous starch microspheres was synthesized in final by two-steps crosslinking with the microporous starch via the method of inverse emulsion polymerization. After that, the adsorption properties of products were mearsured. The factors which can affect the adsorption rate of products were investigated in systematically. According to the results, the reaction conditions were optimized. Besides, the hydrolysis rate was studied in the microporous starch synthesizing process. After the products of crosslinked microporous starch prepared, the crosslinking degree and freeze-thaw stability of them were investigated. Finally, the adsorption properties of crosslinked microporous starch microspheres were studied with nicotine. The main results were summarized as follows:
1. The microporous starch was obtained by enzymatic hydrolysis reaction. During the process, the main reaction conditions which are expected to affect adsorption rate of the products were investigated systematically, including mα-amylase/mglucoamylase, menzyme/mstarch, Vsolution/mstarch, pH, temperature and time of enzymatic reaction. According to the results, the optimal reaction conditions were obtained. Moreover, the hydrolysis rates in each reaction conditions were studied to realize the relationship between the hydrolysis rates and adsorption rates. FTIR was used to compare the structural differences between the native corn starch and microporous starch. SEM images displayed the morphology changes after the treatment with enzyme. The results of XRD showed the changes in crystallinity. DSC determined that the variation of gelatinization temperature.
2. The crosslinked microporous starch was prepared by crosslinking with the microporous starch, which obtained by last step. The effect of each reaction condition on adsorption rate of the products is studied systematically, which included NaOH/mstarch, reaction temperature and time of alkalization, VECH/mstarch, h, pH, reaction temperature and time of crosslinking. The optimal reaction conditions were obtained. FTIR spectra showed the characteristic peaks of the crosslinked microporous starch. And SEM photos revealed its surface morphology.
3. The performance of crosslinked microporous starch prepared by last step was investigated. The relationships among each reaction condition, crosslinking degree of the products, and freeze-thaw stability were studied, In order to study that the changes in crystallinity, the native corn starch and crosslinked microporous starch were examined by XRD. DSC traces showed the alteration in gelatinization temperature.
4. The crosslinked microporous starch microspheres was synthesized by two-steps crosslinking with the microporous starch via the method of inverse emulsion polymerization. The influence of reaction conditions to adsorption rate of the products, such as the different emulsifier (span 60, span 80, tween 60, tween 80), Vcyclohexane/Vsolution, mspan 60/mtween 80?,memulsifie/Vcyclohexane, mstarch/Vsolution, mNNMBA/mstarch, mCAN/mstarch, temperature and time of the crosslinking reaction with NNMBA, h, temperature and time of the crosslinking reaction with ECH, were investigated. The optimal reaction conditions about this method were obtained. Besides, the samples were characterized by FTIR, SEM, XRD and DSC.
5. The experiments for absorbing nicotine of crosslinked microporous starch microspheres were conducted. According to the results, the adsorption kinetics and thermodynamics in this process were investigated. polymerization; adsorption rate; hydrolysis rate; settlement volume; adsorption nicotine; adsorption kinetics; adsorption thermodynamics
引文
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