海藻酸钙凝胶体系中无机矿物（碳酸钙、草酸钙）的结晶行为
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摘要
海藻酸钙水凝胶是一种含有大量水的交联网状物,可用作碳酸钙(CaCO3)和草酸钙(CaC2O4)仿生矿化的前驱体,论文共分为两个部分：
碳酸钙：通过氨和二氧化碳气体的缓慢扩散,海藻酸钙前驱凝胶明确的空间结构、渗透性和离子交换性有利于方解石超结构的形成。当海藻酸钙水凝胶胶凝了大量的液体时,通过对海绵状凝胶珠外部的羧基官能团的成核点的复制,得到了外部方解石排列的碳酸钙。这些方解石超结构的内部特征表明了方解石向内生长的趋势,此即凝胶珠的渗透性和渗透气体的扩散方向。在较少量液体存在(即成核点密度较大)时,前驱凝胶有利于具有平滑表面的方解石超结构的形成,证明了超结构内部方解石纳米颗粒的局部有序排列。这在一定程度上模拟了生物机体控制无机物矿化过程,主要体现在以下几个方面：(1)生物分子官能团吸附Ca2+；(2)三维网状有机结构中的无机矿物的受限结晶；(3)与有机基质结构相关的矿物粒子超结构的形成。此部分最有创新型的研究结果是：一些看上去类似单晶的碳酸钙实际上是由一些微小的方解石斜方颗粒组成的,而且这些堆积的颗粒是沿着聚合物骨架排列的。所以说,多价金属凝胶相中无机矿物的结晶行为为仿生合成功能材料提供了一种新的途径。
草酸钙：草酸钙有一水草酸钙(COM)、二水草酸钙(COD)和三水草酸钙(COT)三种晶型,其中COM是泌尿系统结石的主要组分,与COM相比,COD晶体更容易通过代谢排出。在30℃条件下,草酸铵((NH)4C2O4)饱和溶液加入到不同的钙离子溶液体系中反应得到了形貌和晶型各异的草酸钙沉淀。(1)在水溶液反应体系和邻苯二甲酸氢钾缓冲液反应体系中,当钙离子浓度为0.0172mol／L,改变草酸根的浓度时仅得到相貌各异的COM晶体。(2)在四硼酸钠缓冲液反应体系(固定Ca2+浓度为0.0172 mol／L)中,C2O42-浓度较低时得到的沉淀主要是COD,其中COD的百分含量随着草酸根浓度的增加而降低；C2O42-浓度较高时,得到的沉淀只有COM。(3)(NH)4C2O4饱和溶液与海藻酸钙凝胶混合,反应主要得到了一些球形的聚集结构,其组成单元是多分散的草酸钙晶体颗粒。在Ca2+浓度较低的反应体系中,COM和COD共存；当Ca2+浓度较高时,得到的草酸钙均为COM。固定海藻酸钙水凝胶的量(反应体系中Ca2+浓度约为0.0172 mol／L)时,改变草酸根的浓度得到了COM和COD两种晶型；COD的百分含量随着草酸根浓度的增加而降低,C2O42-浓度较高时,得到的沉淀只有COM。这部分的研究结果表明：在非凝胶反应体系中,四硼酸钠缓冲液能够促进COD的成核与生长；在凝胶反应体系中,海藻酸钙水凝胶不仅能够促进COD的成核与生长,还在草酸钙晶体颗粒聚集结构的形成起到一定的模板作用。
Hydrogels of calcium alginate are the physically cross-linked networks containing a large fraction of water, which could be used as the precursors for the biomimetic mineralization of calcium carbonate (CaCO3) and calcium oxalate (CaC2O4) crystals. Also, these are the main subjects of the thesis.
CaCO3:The well-defined geometry, the permeability, and the ion-exchange property of calcium alginate pre-gels favored the facile fabrication of calcite superstructures through the slow inpouring of ammonia and carbon dioxide gases. This strategic approach indicated to a great extent the biologically controlled mineralization mechanism, dealing with (1) the pre-adsorption of calcium ions by the functional groups of biomolecules, (2) the confined crystallization within the three-dimensional networks, and (3) the proper arrangement of nanosized calcites by association with the organic architectures. Surprisingly, even the apparently 'single-crystalline' CaCO3 was proven to comprise tiny calcite rhombohedrons, furthermore these building blocks co-aligned each other with respect to the polymers' conjugated backbones. Therefore, these suggest a novel pathway of multivalent metal pre-gelation phases for the biomimetic fabrication of functional materials.
CaC2O4:Calcium oxalate crystals have three hydrate forms:calcium oxalate monohydrate (COM), calcium oxalate dihydrate (COD), and calcium oxalate trihydrate (COT), among which COM is the principal inorganic component of urinary deposites and the other two can be easily excreted through urethra. In the in vitro experiments, calcium oxalate crystals were prepared from the mixture of calcium chloride (CaCl2) and ammonium oxalate ((NH4)2C2O4) in different reaction systems at 30℃Only the sheet-like aggregates of COM were precipitated from aqueous systems at various pH values and at a fixed Ca2+concentration of 0.0172 mol/L, so did the reaction systems of the buffer solutions of potassium hydrogen phthalate (pH=4.00). Surprisingly, when Ca2+(0.0172 mol/L) and different amount of C2O42- were added into the buffer solutions of sodium tetraborate (pH=9.18), both COM and COD crystals were obtained at a relatively low concentration of C2O42-. The content of COD decreased with the increase of C2O42- concentration until it disappeared at a relatively high C2O42- concentration.
When calcium alginate hydrogels were used as calcium sources, its reaction with (NH4)2C2O4 resulted in spherical aggerates of calcium oxalate crystals. Crystallographic analyses proved that COM and COD coexisted at a relatively low concentration of Ca2+ions. For example, when Ca2+concentration was fixed at a value of 0.0172 mol/L, the 1:1 molar ratio of Ca2+/C2O42-resulted in the major COD (64.0%) and minor COM (36.0%). The content of COD decreased with the increase of C2O42-, and the unique crystals of COM were obtained at a relatively high concentration of C2O42-ions.
In conclusion, the above results indicated:(1) the supersaturation at a relatively high concentration of Ca2+or C2O42-ions promoted the nucleation and crystallization of COM; (2) sodium tetraborate buffer reaction systems contributed to the formation of COD crystals at a relatively low concentration of C2O42- ions; (3) calcium alginate hydrogels exerted a great influence on the crystallization of COD and played an important role in the template formation of CaC2O4 crystalline superstructures. Interestingly, the formation of COD suggests a biomimetic pathway for the therapy of urinary stones.
碳酸钙：通过氨和二氧化碳气体的缓慢扩散,海藻酸钙前驱凝胶明确的空间结构、渗透性和离子交换性有利于方解石超结构的形成。当海藻酸钙水凝胶胶凝了大量的液体时,通过对海绵状凝胶珠外部的羧基官能团的成核点的复制,得到了外部方解石排列的碳酸钙。这些方解石超结构的内部特征表明了方解石向内生长的趋势,此即凝胶珠的渗透性和渗透气体的扩散方向。在较少量液体存在(即成核点密度较大)时,前驱凝胶有利于具有平滑表面的方解石超结构的形成,证明了超结构内部方解石纳米颗粒的局部有序排列。这在一定程度上模拟了生物机体控制无机物矿化过程,主要体现在以下几个方面：(1)生物分子官能团吸附Ca2+；(2)三维网状有机结构中的无机矿物的受限结晶；(3)与有机基质结构相关的矿物粒子超结构的形成。此部分最有创新型的研究结果是：一些看上去类似单晶的碳酸钙实际上是由一些微小的方解石斜方颗粒组成的,而且这些堆积的颗粒是沿着聚合物骨架排列的。所以说,多价金属凝胶相中无机矿物的结晶行为为仿生合成功能材料提供了一种新的途径。
草酸钙：草酸钙有一水草酸钙(COM)、二水草酸钙(COD)和三水草酸钙(COT)三种晶型,其中COM是泌尿系统结石的主要组分,与COM相比,COD晶体更容易通过代谢排出。在30℃条件下,草酸铵((NH)4C2O4)饱和溶液加入到不同的钙离子溶液体系中反应得到了形貌和晶型各异的草酸钙沉淀。(1)在水溶液反应体系和邻苯二甲酸氢钾缓冲液反应体系中,当钙离子浓度为0.0172mol／L,改变草酸根的浓度时仅得到相貌各异的COM晶体。(2)在四硼酸钠缓冲液反应体系(固定Ca2+浓度为0.0172 mol／L)中,C2O42-浓度较低时得到的沉淀主要是COD,其中COD的百分含量随着草酸根浓度的增加而降低；C2O42-浓度较高时,得到的沉淀只有COM。(3)(NH)4C2O4饱和溶液与海藻酸钙凝胶混合,反应主要得到了一些球形的聚集结构,其组成单元是多分散的草酸钙晶体颗粒。在Ca2+浓度较低的反应体系中,COM和COD共存；当Ca2+浓度较高时,得到的草酸钙均为COM。固定海藻酸钙水凝胶的量(反应体系中Ca2+浓度约为0.0172 mol／L)时,改变草酸根的浓度得到了COM和COD两种晶型；COD的百分含量随着草酸根浓度的增加而降低,C2O42-浓度较高时,得到的沉淀只有COM。这部分的研究结果表明：在非凝胶反应体系中,四硼酸钠缓冲液能够促进COD的成核与生长；在凝胶反应体系中,海藻酸钙水凝胶不仅能够促进COD的成核与生长,还在草酸钙晶体颗粒聚集结构的形成起到一定的模板作用。
Hydrogels of calcium alginate are the physically cross-linked networks containing a large fraction of water, which could be used as the precursors for the biomimetic mineralization of calcium carbonate (CaCO3) and calcium oxalate (CaC2O4) crystals. Also, these are the main subjects of the thesis.
CaCO3:The well-defined geometry, the permeability, and the ion-exchange property of calcium alginate pre-gels favored the facile fabrication of calcite superstructures through the slow inpouring of ammonia and carbon dioxide gases. This strategic approach indicated to a great extent the biologically controlled mineralization mechanism, dealing with (1) the pre-adsorption of calcium ions by the functional groups of biomolecules, (2) the confined crystallization within the three-dimensional networks, and (3) the proper arrangement of nanosized calcites by association with the organic architectures. Surprisingly, even the apparently 'single-crystalline' CaCO3 was proven to comprise tiny calcite rhombohedrons, furthermore these building blocks co-aligned each other with respect to the polymers' conjugated backbones. Therefore, these suggest a novel pathway of multivalent metal pre-gelation phases for the biomimetic fabrication of functional materials.
CaC2O4:Calcium oxalate crystals have three hydrate forms:calcium oxalate monohydrate (COM), calcium oxalate dihydrate (COD), and calcium oxalate trihydrate (COT), among which COM is the principal inorganic component of urinary deposites and the other two can be easily excreted through urethra. In the in vitro experiments, calcium oxalate crystals were prepared from the mixture of calcium chloride (CaCl2) and ammonium oxalate ((NH4)2C2O4) in different reaction systems at 30℃Only the sheet-like aggregates of COM were precipitated from aqueous systems at various pH values and at a fixed Ca2+concentration of 0.0172 mol/L, so did the reaction systems of the buffer solutions of potassium hydrogen phthalate (pH=4.00). Surprisingly, when Ca2+(0.0172 mol/L) and different amount of C2O42- were added into the buffer solutions of sodium tetraborate (pH=9.18), both COM and COD crystals were obtained at a relatively low concentration of C2O42-. The content of COD decreased with the increase of C2O42- concentration until it disappeared at a relatively high C2O42- concentration.
When calcium alginate hydrogels were used as calcium sources, its reaction with (NH4)2C2O4 resulted in spherical aggerates of calcium oxalate crystals. Crystallographic analyses proved that COM and COD coexisted at a relatively low concentration of Ca2+ions. For example, when Ca2+concentration was fixed at a value of 0.0172 mol/L, the 1:1 molar ratio of Ca2+/C2O42-resulted in the major COD (64.0%) and minor COM (36.0%). The content of COD decreased with the increase of C2O42-, and the unique crystals of COM were obtained at a relatively high concentration of C2O42-ions.
In conclusion, the above results indicated:(1) the supersaturation at a relatively high concentration of Ca2+or C2O42-ions promoted the nucleation and crystallization of COM; (2) sodium tetraborate buffer reaction systems contributed to the formation of COD crystals at a relatively low concentration of C2O42- ions; (3) calcium alginate hydrogels exerted a great influence on the crystallization of COD and played an important role in the template formation of CaC2O4 crystalline superstructures. Interestingly, the formation of COD suggests a biomimetic pathway for the therapy of urinary stones.
引文
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