多孔二氧化硅系材料的制备与性能研究
摘要
合成了具有发散性介孔孔道结构的荧光二氧化硅纳米颗粒（FMSN）。研究了FMSN的生长过程，TEM结果表明随着反应时间的延长，颗粒之间的二氧化硅连接体的作用变弱导致二氧化硅纳米颗粒的形成，反应时间为3h时是最优化的反应时间。研究了荧光基团（APTES-SA，氨基丙基三乙氧基硅烷-水杨酸）和催化剂（TEA，三乙醇胺）对FMSN的影响，结果表明随着TEOS（正硅酸乙酯）与TEA的摩尔比的降低，FMSN的颗粒尺寸增大，随着APTES-SA的加入量的增加，颗粒尺寸增大，同时颗粒变得更致密。太多的APTES-SA（APTES-SA/TEOS=0.4）将会导致整片二氧化硅的形成。FMSN的荧光性质通过吸收和发射光谱测试获得，结果表明荧光基团完全加载到了二氧化硅上，没有游离地存在于液体中。
在室温下快速合成了具有发散性定向孔道结构的中空二氧化硅材料（ROPHS）。研究了DMF（N-N二甲基甲酰胺）的加入量对其形成过程的影响，TEM结果表明当DMF的加入量为零或很少时，只形成了实心纳米二氧化硅颗粒。然而，随着DMF的加入量的增加，中空结构逐渐形成。研究了反应时间对ROPHS生长过程的影响，结果表明，中空二氧化硅材料可以在很短的时间内形成，即只需要0.5h，并且此时实心的二氧化硅纳米颗粒还没有形成。随着反应时间的延长，孔道结构部分的厚度增加。当用超声代替搅拌时，发现中空二氧化硅材料的总的尺寸和中空部分的尺寸均有所减小。TEM观察显示，Au和Fe3O4纳米颗粒均可被包裹于中空部分形成核壳结构，在药物释放领域具有潜在的应用价值。
研究了ZSM-5、Silicalite-1和Zeolite Y分子筛材料的合成以及通过TGA测试研究了其在吸附CO_2方面的性能。通过水热反应法合成了尺寸均匀的ZSM-5分子筛材料，并对其进行了离子交换处理。尺寸均匀的Silicalite-1通过回流加热的方法制得。合成了具有纯相结构的Zeolite Y分子筛材料，并对其进行了离子交换处理。TGA结果表明：ZSM-5（AS2）、Na（Ⅰ）-ZSM-5（AS2）、 Na（Ⅱ）-ZSM-5（AS2）、 Na（Ⅰ）-CBV2314、Na（Ⅱ）-CBV2314、 Na（Ⅱ）-CBV8014、 Silicalite-1-500-10、 Na（Ⅰ）-Y、 Na（Ⅱ）-Y、 La（Ⅰ）-Na（Ⅰ）-Y、 Mg（Ⅰ）-Na（Ⅰ）-Y和NaY分别可以吸附0.5%、2.3%、5.0%、1.9%、2.5%、3.6%、3.4%、3.6%、4.0%、2.0%、2.5%和3.4%的CO_2。本实验研究的所有分子筛材料中，Na（II）-ZSM-5（AS2）吸附CO_2的能力最强。
Fluorescent mesoporous silica nanoparticles (FMSN) with radialmesochannels were synthesized. The growth process of FMSN was studied.TEM results indicated that with the extension of reaction time, the effect ofsilica connectors between particles was weakened, resulting in theformation of silica nanoparticles. The optimal reaction time was3h. Theeffects of fluorescent groups (APTES-SA,Aminopropyltriethoxysilane-Salicylic Acid) and catalyst (TEA,Triethanolamine) on the FMSN were investigated, suggesting that withdecreasing the molar ratio of TEOS (Tetraethyl Orthosilicate)/TEA, theparticle size of FMSN increased. Meanwhile, as the addition of APTES-SA,the particle size increased and the particles became more compaction. Buttoo much APTES (APTES-SA/TEOS=0.4) resulted in the formation ofwhole piece of silica. The fluorescent properties of FMSN were studied bythe absorption and emission spectra, revealing that all fluorescent groupswere linked to the silica particles.
The hollow porous silica particles with radially oriented porous wall(ROPHS) were synthesized at room temperature by an instant method. Theeffect of DMF (N,N-dimethylformide) on the formation of ROPHS wasstudied. When zero or small amount of DMF was added, pure solid silicananoparticles were obtained by TEM. However, with the increase of theaddition of DMF, more hollow silica particles were formed. Moreover, thethickness of the wall kept the same in each condition. The effects ofdifferent reaction time on the growth process of ROPHS were studied,indicating that hollow porous silica can be formed instantly, only in0.5h. At the same time, the solid mesoporous silica was not formed. With theincrease of reaction time, the thickness of the porous wall increased. Whenchanging stirring to sonication, the total size and the hollow phase size ofporous silica decreasd. TEM observation showed that Au and Fe3O4nanoparticles could be totally trapped into porous silica to form core-shellstructure, which has the potential application in drug release.
ZSM-5, silicalite-1and zeolite Y materials were synthesized and itsCO_2adsorption performance was carried out by TGA method. HomogenousZSM-5crystals were synthesized by hydrothermal treatment and treated byion exchange. Homegeneous silicalite-1particles were synthesized byreflux heating treatment. Pure zeolite Y material was synthesized andtreated by ion exchange. According to the TGA results, CO_2pickupcapacities of ZSM-5(AS2), Na(Ⅰ)-ZSM-5(AS2), Na(Ⅱ)-ZSM-5(AS2),Na(Ⅰ)-CBV2314, Na(Ⅱ)-CBV2314, Na(Ⅱ)-CBV8014, silicalite-1-500-10,Na(Ⅰ)-Y, Na(Ⅱ)-Y, La(Ⅰ)-Na(Ⅰ)-Y, Mg(Ⅰ)-Na(Ⅰ)-Y and NaY are0.5%,2.3%,5.0%,1.9%,2.5%,3.6%,3.4%,3.6%,4.0%,2.0%,2.5%and3.4%,respectively. Among all zeolite samples studied in this work, CO_2pickupcapacity of Na(Ⅱ)-ZSM-5(AS2) was the highest.
在室温下快速合成了具有发散性定向孔道结构的中空二氧化硅材料（ROPHS）。研究了DMF（N-N二甲基甲酰胺）的加入量对其形成过程的影响，TEM结果表明当DMF的加入量为零或很少时，只形成了实心纳米二氧化硅颗粒。然而，随着DMF的加入量的增加，中空结构逐渐形成。研究了反应时间对ROPHS生长过程的影响，结果表明，中空二氧化硅材料可以在很短的时间内形成，即只需要0.5h，并且此时实心的二氧化硅纳米颗粒还没有形成。随着反应时间的延长，孔道结构部分的厚度增加。当用超声代替搅拌时，发现中空二氧化硅材料的总的尺寸和中空部分的尺寸均有所减小。TEM观察显示，Au和Fe3O4纳米颗粒均可被包裹于中空部分形成核壳结构，在药物释放领域具有潜在的应用价值。
研究了ZSM-5、Silicalite-1和Zeolite Y分子筛材料的合成以及通过TGA测试研究了其在吸附CO_2方面的性能。通过水热反应法合成了尺寸均匀的ZSM-5分子筛材料，并对其进行了离子交换处理。尺寸均匀的Silicalite-1通过回流加热的方法制得。合成了具有纯相结构的Zeolite Y分子筛材料，并对其进行了离子交换处理。TGA结果表明：ZSM-5（AS2）、Na（Ⅰ）-ZSM-5（AS2）、 Na（Ⅱ）-ZSM-5（AS2）、 Na（Ⅰ）-CBV2314、Na（Ⅱ）-CBV2314、 Na（Ⅱ）-CBV8014、 Silicalite-1-500-10、 Na（Ⅰ）-Y、 Na（Ⅱ）-Y、 La（Ⅰ）-Na（Ⅰ）-Y、 Mg（Ⅰ）-Na（Ⅰ）-Y和NaY分别可以吸附0.5%、2.3%、5.0%、1.9%、2.5%、3.6%、3.4%、3.6%、4.0%、2.0%、2.5%和3.4%的CO_2。本实验研究的所有分子筛材料中，Na（II）-ZSM-5（AS2）吸附CO_2的能力最强。
Fluorescent mesoporous silica nanoparticles (FMSN) with radialmesochannels were synthesized. The growth process of FMSN was studied.TEM results indicated that with the extension of reaction time, the effect ofsilica connectors between particles was weakened, resulting in theformation of silica nanoparticles. The optimal reaction time was3h. Theeffects of fluorescent groups (APTES-SA,Aminopropyltriethoxysilane-Salicylic Acid) and catalyst (TEA,Triethanolamine) on the FMSN were investigated, suggesting that withdecreasing the molar ratio of TEOS (Tetraethyl Orthosilicate)/TEA, theparticle size of FMSN increased. Meanwhile, as the addition of APTES-SA,the particle size increased and the particles became more compaction. Buttoo much APTES (APTES-SA/TEOS=0.4) resulted in the formation ofwhole piece of silica. The fluorescent properties of FMSN were studied bythe absorption and emission spectra, revealing that all fluorescent groupswere linked to the silica particles.
The hollow porous silica particles with radially oriented porous wall(ROPHS) were synthesized at room temperature by an instant method. Theeffect of DMF (N,N-dimethylformide) on the formation of ROPHS wasstudied. When zero or small amount of DMF was added, pure solid silicananoparticles were obtained by TEM. However, with the increase of theaddition of DMF, more hollow silica particles were formed. Moreover, thethickness of the wall kept the same in each condition. The effects ofdifferent reaction time on the growth process of ROPHS were studied,indicating that hollow porous silica can be formed instantly, only in0.5h. At the same time, the solid mesoporous silica was not formed. With theincrease of reaction time, the thickness of the porous wall increased. Whenchanging stirring to sonication, the total size and the hollow phase size ofporous silica decreasd. TEM observation showed that Au and Fe3O4nanoparticles could be totally trapped into porous silica to form core-shellstructure, which has the potential application in drug release.
ZSM-5, silicalite-1and zeolite Y materials were synthesized and itsCO_2adsorption performance was carried out by TGA method. HomogenousZSM-5crystals were synthesized by hydrothermal treatment and treated byion exchange. Homegeneous silicalite-1particles were synthesized byreflux heating treatment. Pure zeolite Y material was synthesized andtreated by ion exchange. According to the TGA results, CO_2pickupcapacities of ZSM-5(AS2), Na(Ⅰ)-ZSM-5(AS2), Na(Ⅱ)-ZSM-5(AS2),Na(Ⅰ)-CBV2314, Na(Ⅱ)-CBV2314, Na(Ⅱ)-CBV8014, silicalite-1-500-10,Na(Ⅰ)-Y, Na(Ⅱ)-Y, La(Ⅰ)-Na(Ⅰ)-Y, Mg(Ⅰ)-Na(Ⅰ)-Y and NaY are0.5%,2.3%,5.0%,1.9%,2.5%,3.6%,3.4%,3.6%,4.0%,2.0%,2.5%and3.4%,respectively. Among all zeolite samples studied in this work, CO_2pickupcapacity of Na(Ⅱ)-ZSM-5(AS2) was the highest.
引文
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