微孔淀粉材料优化制备技术及其应用研究
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摘要
微孔淀粉是一种有大量微孔的、来源天然、经济易得的物质,由于其具有较大的比表面积、比孔容而具有良好的吸附性能,可广泛应用于食品、医药、化妆品、农业等领域。它的制备方法主要有低于糊化温度酶解法、高温泡沫法、溶剂交换技术法等。
本论文以玉米、木薯、甘薯、豌豆、小麦、马铃薯淀粉为材料,研究了微孔化淀粉和交联化微孔淀粉的工艺路线和参数、研究了微孔淀粉和交联微孔淀粉的显微结构和亲水亲脂吸附特性,研究了糊化冷冻溶剂交换新技术制备小麦微孔淀粉的工艺路线和参数,研究了以微孔淀粉为原料制备精细化工产品超微氧化锌的工艺路线和参数。
1以玉米淀粉制备微孔淀粉的工艺为低于淀粉糊化温度酶解法。最佳工艺参数为：淀粉乳浓度为14.24%,酶用量4%,酶配比(α-淀粉酶：糖化酶)为1：4,缓冲溶液pH值4.4,反应时间13.15h,反应温度51.92℃。
对比了微孔淀粉与原淀粉的理化性质,结果表明：淀粉微孔化后,比表面积、比孔容增大,吸附性能大幅度提高。获得的玉米微孔淀粉颗粒表面布满小孔,形成中空的显微结构特点。与原淀粉相比,吸水率达到143.01%,增长了134.15%。
2微孔淀粉吸附的热力学、动力学研究表明：微孔淀粉对次甲基蓝的吸附符合准二级动力学方程。微孔淀粉对次甲基蓝的吸附符合Freundlich吸附等温方程。体系温度升高,微孔淀粉对次甲基蓝的吸附量逐渐减少说明此过程可能是一放热过程。吸附热力学参数为：△Gθ<0,△Hθ<0,△Sθ<0,吸附是自发的过程。
3对比了6种淀粉微孔化的吸附性能,从大到小的是：玉米淀粉>木薯淀粉>甘薯淀粉>豌豆淀粉。马铃薯、小麦淀粉酶解基本上不能形成孔洞。
小麦淀粉为难酶解和难微孔化淀粉。对小麦淀粉进行了物理预处理后酶解的探索,方法有超高压、紫外照射、超声波处理、退火、冷冻溶剂交换技术处理等,结果表明,这些处理对淀粉颗粒都有不同程度的作用,但是酶解后,仍然不能形成微孔。应用糊化冷冻溶剂交换工艺可制备微孔化小麦淀粉。其工艺技术为：糊化冷冻溶剂交换技术。其较佳工艺为：5g淀粉添加40-50mL水,水浴锅90℃糊化25-30min,降至室温后,放冰箱5℃冷藏48h,最易切块成型。再放入-10℃冷冻48h,以乙醇：水=10：0比例浸没3次,干燥后得到的小麦淀粉多孔材料。获得的微孔淀粉多孔材料模板具有孔径均匀的特点。与原淀粉相比,吸水率达到245.66%,增长了300.20%。
4为提高微孔淀粉吸附性能,改变其亲水亲脂吸附特性,增强其抗剪切能力和热稳定性,可采用交联淀粉微孔化工艺。其工艺为先交联后微孔化技术。最佳工艺参数为淀粉乳浓度15%,交联剂用量0.04mL·100g-1,酶用量5%,酶配比(α-淀粉酶：糖化酶)为1：4,缓冲溶液pH值4.4,反应时间12h,反应温度50℃。获得的交联微孔淀粉与微孔淀粉相比,孔径由1.7μm增大到2.4μm,比孔容增大的显微结构特点。与微孔淀粉相比吸水率由143.01%增加到150.97%,吸油能力由1.4mL·g-1增加到1.5mL·g-1,吸附性能得到改善,亲水亲脂吸附特性得到增强。抗剪切能力,冷热稳定性增强,结构得到强化。
5微孔淀粉和交联微孔淀粉具有强吸附性能,可应用于精细化工产品的制备。本研究以微孔化小麦淀粉为模板,制备了超微氧化锌。其工艺为液相法煅烧技术。成功制取了超微氧化锌粉。
Micro-porous starch is a kind of natural, economical and easily accessible material. On account of its large BET surface area, voluminous micro-pores and excellent adsorption capability, micro-porous starch has been widely applied in the field of food, pharmaceuticals, cosmetics, pulp and paper industries, as well as agriculture. The manufacturing methods of micro-porous starch include enzymatic hydrolysis at temperatures below the starch gelatinization temperature, foaming at high temperature and exchanging solvent.
In this dissertation, starches of cassava, sweet potato, corn, peas, wheat and potato were employed as experimental materials, the process route, optimum parameters. micro structure, hydrophilic and lipophilic adsorption property of micro-porous starch and cross-linked starch were investigated. The technological route and optimum parameters of a new technology of processing wheat micro-porous, gelatinization starch by exchanging frozen solvent, were also investigated. The method of processing superfine zinc oxide with micro-porous starch as raw material was explored, and optimum parameters were studied.
1. Corn micro-porous starch was prepared by the method of enzymatic hydrolysis at temperatures below the starch gelatinization temperature. Results indicated that the optimum conditions were starch concentration (V/V)15%, enzyme amount4%, glucoamylase-amylase ratio4:1, buffer pH4.4, reaction time12h and temperature50℃.
By comparison physical and chemical characteristics of micro-porous starch with that of original one, the size and volume of aperture, specific surface area and adsorption capacity of micro-porous starches were greatly improved. The surface of micro-porous maize starch granule was riddled with holes, forming a hollow microstructure after enzymatic hydrolysis. The water-absorption capacity of porous starch amounted to143.01%, increasing by134.15%than original starch.
2. The adsorption thermodynamics and kinetics of the micro-porous starch was studied, and result showed that the adsorption mode of methylene blue by micro-porous starch corresponded well with quasi two level dynamic equation. This adsorption fitted into Freundlich isothermal adsorption equation. When system temperature increased, the amount of adsorbed methylene blue decreased gradually. So it could be inferred that the adsorption process was an exothermic and spontaneous one, with thermodynamic parameters as:ΔGθ<0, ΔHθ<0, ΔSθ<0.
3. The adsorption capacity of six types of starches was compared; the sequence was corn starch, tapioca starch, sweet potato starch, pea starch by descending order. Almost no aperture could form after potato and wheat starch were treated by enzymatic hydrolysis.
Since wheat starch was difficult to be hydrolyzed by enzymes and form porous structure in starch granules, we added physical pretreatment before enzymatic hydrolysis. The pretreatment methods included ultra-high pressure, ultraviolet irradiation, ultrasonic treatment, annealing, cold solvent exchange processing. Results showed that these treatments had different effect on starch granules, but still could not form pores after enzymatic hydrolysis. The micro-porous wheat starch could be processed by gelatinizing, freezing starch, and exchanging solvent.
The optimum process was adding5g starch into40～50mL water, keeping the mixture in a water bath at90℃for25～30min to gelatinize starch, cooling down it to room temperature, storing it in a refrigerator at5℃for48h, cutting it into cubes, freezing it at-10℃for48h, rinsing it with ethanol-water (ratio10:0) for3times, drying it, and the pores forming on the surface of wheat starch granules. So obtained micro-porous wheat starch granules had the merit of uniform pore size, which is desirable for multiple-purpose porous materials. Compared with the original starch, the water-absorbing capacity of porous starch approached to245.66%, increasing by300.20%.
4. In order to improve the adsorption capacity of micro-porous starch, the hydrophilic and lipophilic adsorption was modified, its shear resistance capability and heat stability was improved, and a process of cross-linking and enzymatic hydrolyzing to make micro pores was employed to treat starch. Results indicated that the optimal preparation parameters were starch concentration (V/V)15%, epichlorohydrin dosage0.04mL/100g, enzyme amount5.0%, glucoamylase-amylase ratio4:1, buffer pH4.4, reaction time12h, temperature50℃. A systematic comparison of the physical and chemical characteristics was made between crosslinked micro-porous starch granule and microporous starch granule. The crosslinked micro-porous starch had larger pore size (2.4μm diameter) than that of micro-porous starch (1.7μm diameter), larger micro-pore volume, greater water-absorption capacity (150.97%) than that of micro-porous starch (143.01%), greater oil-absorption capacity (1.5mL·g-1) than that of micro-porous starch (1.4mL·g-1), so the absorption capacity was greatly improved. The hydrophilic and lipophilic adsorption, resistance to shear action, heat and cold stability, structure of micro pores were also improved.
5. On account of their excellent adsorption capacity, the micro-porous starch and cross-linked porous corn starch could be applied to the preparation of fine chemical products. The paper used wheat starch with micro pores as a template in the preparation of ultrafine zinc oxide. The superfine zinc oxide was successfully processed by a calcination technique carried out in liquid phase, coupled with a powder process.
本论文以玉米、木薯、甘薯、豌豆、小麦、马铃薯淀粉为材料,研究了微孔化淀粉和交联化微孔淀粉的工艺路线和参数、研究了微孔淀粉和交联微孔淀粉的显微结构和亲水亲脂吸附特性,研究了糊化冷冻溶剂交换新技术制备小麦微孔淀粉的工艺路线和参数,研究了以微孔淀粉为原料制备精细化工产品超微氧化锌的工艺路线和参数。
1以玉米淀粉制备微孔淀粉的工艺为低于淀粉糊化温度酶解法。最佳工艺参数为：淀粉乳浓度为14.24%,酶用量4%,酶配比(α-淀粉酶：糖化酶)为1：4,缓冲溶液pH值4.4,反应时间13.15h,反应温度51.92℃。
对比了微孔淀粉与原淀粉的理化性质,结果表明：淀粉微孔化后,比表面积、比孔容增大,吸附性能大幅度提高。获得的玉米微孔淀粉颗粒表面布满小孔,形成中空的显微结构特点。与原淀粉相比,吸水率达到143.01%,增长了134.15%。
2微孔淀粉吸附的热力学、动力学研究表明：微孔淀粉对次甲基蓝的吸附符合准二级动力学方程。微孔淀粉对次甲基蓝的吸附符合Freundlich吸附等温方程。体系温度升高,微孔淀粉对次甲基蓝的吸附量逐渐减少说明此过程可能是一放热过程。吸附热力学参数为：△Gθ<0,△Hθ<0,△Sθ<0,吸附是自发的过程。
3对比了6种淀粉微孔化的吸附性能,从大到小的是：玉米淀粉>木薯淀粉>甘薯淀粉>豌豆淀粉。马铃薯、小麦淀粉酶解基本上不能形成孔洞。
小麦淀粉为难酶解和难微孔化淀粉。对小麦淀粉进行了物理预处理后酶解的探索,方法有超高压、紫外照射、超声波处理、退火、冷冻溶剂交换技术处理等,结果表明,这些处理对淀粉颗粒都有不同程度的作用,但是酶解后,仍然不能形成微孔。应用糊化冷冻溶剂交换工艺可制备微孔化小麦淀粉。其工艺技术为：糊化冷冻溶剂交换技术。其较佳工艺为：5g淀粉添加40-50mL水,水浴锅90℃糊化25-30min,降至室温后,放冰箱5℃冷藏48h,最易切块成型。再放入-10℃冷冻48h,以乙醇：水=10：0比例浸没3次,干燥后得到的小麦淀粉多孔材料。获得的微孔淀粉多孔材料模板具有孔径均匀的特点。与原淀粉相比,吸水率达到245.66%,增长了300.20%。
4为提高微孔淀粉吸附性能,改变其亲水亲脂吸附特性,增强其抗剪切能力和热稳定性,可采用交联淀粉微孔化工艺。其工艺为先交联后微孔化技术。最佳工艺参数为淀粉乳浓度15%,交联剂用量0.04mL·100g-1,酶用量5%,酶配比(α-淀粉酶：糖化酶)为1：4,缓冲溶液pH值4.4,反应时间12h,反应温度50℃。获得的交联微孔淀粉与微孔淀粉相比,孔径由1.7μm增大到2.4μm,比孔容增大的显微结构特点。与微孔淀粉相比吸水率由143.01%增加到150.97%,吸油能力由1.4mL·g-1增加到1.5mL·g-1,吸附性能得到改善,亲水亲脂吸附特性得到增强。抗剪切能力,冷热稳定性增强,结构得到强化。
5微孔淀粉和交联微孔淀粉具有强吸附性能,可应用于精细化工产品的制备。本研究以微孔化小麦淀粉为模板,制备了超微氧化锌。其工艺为液相法煅烧技术。成功制取了超微氧化锌粉。
Micro-porous starch is a kind of natural, economical and easily accessible material. On account of its large BET surface area, voluminous micro-pores and excellent adsorption capability, micro-porous starch has been widely applied in the field of food, pharmaceuticals, cosmetics, pulp and paper industries, as well as agriculture. The manufacturing methods of micro-porous starch include enzymatic hydrolysis at temperatures below the starch gelatinization temperature, foaming at high temperature and exchanging solvent.
In this dissertation, starches of cassava, sweet potato, corn, peas, wheat and potato were employed as experimental materials, the process route, optimum parameters. micro structure, hydrophilic and lipophilic adsorption property of micro-porous starch and cross-linked starch were investigated. The technological route and optimum parameters of a new technology of processing wheat micro-porous, gelatinization starch by exchanging frozen solvent, were also investigated. The method of processing superfine zinc oxide with micro-porous starch as raw material was explored, and optimum parameters were studied.
1. Corn micro-porous starch was prepared by the method of enzymatic hydrolysis at temperatures below the starch gelatinization temperature. Results indicated that the optimum conditions were starch concentration (V/V)15%, enzyme amount4%, glucoamylase-amylase ratio4:1, buffer pH4.4, reaction time12h and temperature50℃.
By comparison physical and chemical characteristics of micro-porous starch with that of original one, the size and volume of aperture, specific surface area and adsorption capacity of micro-porous starches were greatly improved. The surface of micro-porous maize starch granule was riddled with holes, forming a hollow microstructure after enzymatic hydrolysis. The water-absorption capacity of porous starch amounted to143.01%, increasing by134.15%than original starch.
2. The adsorption thermodynamics and kinetics of the micro-porous starch was studied, and result showed that the adsorption mode of methylene blue by micro-porous starch corresponded well with quasi two level dynamic equation. This adsorption fitted into Freundlich isothermal adsorption equation. When system temperature increased, the amount of adsorbed methylene blue decreased gradually. So it could be inferred that the adsorption process was an exothermic and spontaneous one, with thermodynamic parameters as:ΔGθ<0, ΔHθ<0, ΔSθ<0.
3. The adsorption capacity of six types of starches was compared; the sequence was corn starch, tapioca starch, sweet potato starch, pea starch by descending order. Almost no aperture could form after potato and wheat starch were treated by enzymatic hydrolysis.
Since wheat starch was difficult to be hydrolyzed by enzymes and form porous structure in starch granules, we added physical pretreatment before enzymatic hydrolysis. The pretreatment methods included ultra-high pressure, ultraviolet irradiation, ultrasonic treatment, annealing, cold solvent exchange processing. Results showed that these treatments had different effect on starch granules, but still could not form pores after enzymatic hydrolysis. The micro-porous wheat starch could be processed by gelatinizing, freezing starch, and exchanging solvent.
The optimum process was adding5g starch into40～50mL water, keeping the mixture in a water bath at90℃for25～30min to gelatinize starch, cooling down it to room temperature, storing it in a refrigerator at5℃for48h, cutting it into cubes, freezing it at-10℃for48h, rinsing it with ethanol-water (ratio10:0) for3times, drying it, and the pores forming on the surface of wheat starch granules. So obtained micro-porous wheat starch granules had the merit of uniform pore size, which is desirable for multiple-purpose porous materials. Compared with the original starch, the water-absorbing capacity of porous starch approached to245.66%, increasing by300.20%.
4. In order to improve the adsorption capacity of micro-porous starch, the hydrophilic and lipophilic adsorption was modified, its shear resistance capability and heat stability was improved, and a process of cross-linking and enzymatic hydrolyzing to make micro pores was employed to treat starch. Results indicated that the optimal preparation parameters were starch concentration (V/V)15%, epichlorohydrin dosage0.04mL/100g, enzyme amount5.0%, glucoamylase-amylase ratio4:1, buffer pH4.4, reaction time12h, temperature50℃. A systematic comparison of the physical and chemical characteristics was made between crosslinked micro-porous starch granule and microporous starch granule. The crosslinked micro-porous starch had larger pore size (2.4μm diameter) than that of micro-porous starch (1.7μm diameter), larger micro-pore volume, greater water-absorption capacity (150.97%) than that of micro-porous starch (143.01%), greater oil-absorption capacity (1.5mL·g-1) than that of micro-porous starch (1.4mL·g-1), so the absorption capacity was greatly improved. The hydrophilic and lipophilic adsorption, resistance to shear action, heat and cold stability, structure of micro pores were also improved.
5. On account of their excellent adsorption capacity, the micro-porous starch and cross-linked porous corn starch could be applied to the preparation of fine chemical products. The paper used wheat starch with micro pores as a template in the preparation of ultrafine zinc oxide. The superfine zinc oxide was successfully processed by a calcination technique carried out in liquid phase, coupled with a powder process.
引文
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