論文 - 中西　和樹

Fabrication process development and basic evaluation of eggshell-based column packing material for reversed-phase preparative separation 査読有り

Yoshii Tomoka, Sakama Akihiro, Kanamori Kazuyoshi, Nakanishi Kazuki, Imai Hiroaki, Citterio Daniel, Hiruta Yuki

JOURNAL OF CHROMATOGRAPHY A   1688 巻   頁： 463722   2023年1月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Journal of Chromatography A  

Purification of basic drugs in reversed-phase mode is often difficult, mainly due to adsorption of positively charged compounds to the silica gel-based stationary phase. Since this adsorption can be suppressed under alkaline condition, columns with alkali-resistance are required. In addition, compounds with acid-sensitive structures are sometimes degraded during separation on silica gel-based columns which exhibit acidity due to their surface structure. We prepared an alkali-resistant reversed-phase packing material, Eggshell-PMAcO based on eggshells modified with an amphiphilic copolymer, poly(maleic acid-alt-1-octadecene) (PMAcO). The height equivalent to a theoretical plate (HETP) of the Eggshell-PMAcO column was improved by surface treatment with ammonium acetate buffer (900 mM, pH = 3.7), which is an inexpensive reagent, and the retention behavior for hydrophobic compounds was compared to a typical ODS column based on silica gel, resulting in sufficient selectivity of the eggshell-based column for hydrophobic compounds, as indicated by the ratio of retention factors of pentylbenzene and butylbenzene (Eggshell-PMAcO column: 1.55, ODS column: 1.65). Column temperature-dependent retention behavior of naphthalene was investigated in the temperature range from 25 °C to 45 °C, followed by the calculation of thermodynamic parameters. There was little difference in the standard molar enthalpy (Eggshell-PMAcO: −19.6 kJ/mol, ODS: −21.7 kJ/mol). The absolute value of the standard free Gibbs energy for the Eggshell-PMAcO column was much smaller than that of the ODS column (Eggshell-PMAcO: −0.284 kJ/mol, ODS: −13.0 kJ/mol), indicating that the Eggshell-PMAcO column had a weaker retention strength for naphthalene than the ODS column mainly due to the large difference in the standard molar entropy (Eggshell-PMAcO: −64.9 J/mol K, ODS column: −29.2 J/mol K). The retention capacities for imipramine under neutral (water/methanol) and alkaline (0.1% triethylamine water/methanol) conditions were 0.2 mg and 5 mg, respectively, based on injection mass-dependent HETP, retention factor and symmetry factor. Finally, the prepared column was applied to the purification of a building block for nucleic acid drugs. This study demonstrated that reversed-phase columns, which can be fabricated from eggshells and an amphiphilic copolymer in an inexpensive and eco-friendly way, have the ability to purify basic compounds and acid-sensitive compounds.

DOI： 10.1016/j.chroma.2022.463722

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Macroporous Niobium Phosphate-Supported Magnesia Catalysts for Isomerization of Glucose-to-Fructose 査読有り

Gao Da-Ming, Shen Yong-Bing, Zhao Bohan, Liu Qian, Nakanishi Kazuki, Chen Jie, Kanamori Kazuyoshi, Wu Huaping, He Zhiyong, Zeng Maomao, Liu Haichao

ACS SUSTAINABLE CHEMISTRY & ENGINEERING   7 巻 ( 9 ) 頁： 8512 - 8521   2019年5月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：ACS Sustainable Chemistry and Engineering  

The catalytic performance of hierarchically porous niobium phosphate (NbP) supported magnesia for the glucose isomerization to fructose, was investigated under atmospheric air atmosphere. Porous NbP showed improved support effects on MgO in comparison to other metal oxides tested for glucose isomerization. Also, the amount and distribution of basic sites were largely changed by supporting magnesia on NbP. Although the textural properties were reduced and solid acids formed on the MgO/NbP catalysts, glucose isomerization was promoted by increasing magnesium content. The maximum yield of fructose reached ∼24.6% over 40%MgO/NbP-500 with selectivity of 65.7% for 1.0 wt % glucose at 120 °C. The fructose productivity peaked as high as 13.6 g g catalyst-1 h -1 over 40%MgO/NbP-700 catalyst. The leaching of cations and anions resulted in a homogeneous system for glucose isomerization. Regeneration almost fully reactivated the catalyst to its initial activity. The MgO/NbP showed high stability under air atmosphere for 15 days, and high potential use for glucose isomerization.

DOI： 10.1021/acssuschemeng.9b00292

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Hierarchically Porous Monoliths of Oxygen-deficient Anatase TiO2-x with Electronic Conductivity (vol 3, pg 7205, 2013) 査読有り

Kitada Atsushi, Hasegawa George, Kobayashi Yoji, Miyazaki Kohei, Abe Takeshi, Kanamori Kazuyoshi, Nakanishi Kazuki, Kageyama Hiroshi

RSC ADVANCES   3 巻 ( 48 ) 頁： 26475 - 26475   2013年

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記述言語：英語   掲載種別：研究論文（学術雑誌）  

Web of Science

Elastic Aerogels and Xerogels Synthesized From Methyltrimethoxysilane (MTMS) 査読有り

Kanamori Kazuyoshi, Nakanishi Kazuki, Hanada Teiichi

POLYMER-BASED SMART MATERIALS - PROCESSES, PROPERTIES AND APPLICATION   1134 巻   頁： 173 - +   2009年

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記述言語：英語   掲載種別：研究論文（学術雑誌）  

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Examination of mesopore structure of hierarchically macro/mesoporous silica by thermoporometry 査読有り

Fukui E., Shinohara K., Nakanishi K., Kanamori K., Hanada T.

Materials Research Society Symposium Proceedings   1056 巻   頁： 28 - 33   2008年12月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Materials Research Society Symposium Proceedings  

Thermoporometry was employed to monitor the mesopore evolution in wet, drying and heat-treatment stages of monolithic macro/mesoporous silica with SBA-15 like structure. Direct comparison of mesopores in wet state was only possible with the samples extracted with sulfuric acid. In good agreement with the preceding study, the sulfuric acid not only removed the surfactant but also modified the silica gel network into that with reduced amount of micropores and increased stability against the drying stress. Thermoporometry revealed that the structural evolution takes place completely in the wet condition, which accompanies a decrease in the thickness of non-freezable water. © 2008 Materials Research Society.

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Hierarchically porous oxides, hybrids and polymers via sol-gel accompanied by phase separation 査読有り

Nakanishi K.

Materials Research Society Symposium Proceedings   1007 巻   頁： 51 - 62   2008年9月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Materials Research Society Symposium Proceedings  

In various crosslinking systems containing metal oxides, organo-siloxane polymers and pure hydrocarbons, monolithic materials with hierarchical well-defined macropores and controlled mesopores have been synthesized. Synthetic progress in alkoxy-derived macroporous silica lead to the preparation of long-range ordered mesoporous skeletons in well-defined macroporous framework. Alkylene-bridged silicon alkoxides can also be prepared into similarly hierarchical porous structures with broadened variations in framework morphology. Macro-mesoporous alkoxy-derived pure titania and zirconia have been prepared using hydrochloric acid - mediated processes. Compared with those prepared from colloidal dispersions, alkoxy-derived macroporous titania exhibited much higher mechanical strength. Titania monolith is a promising candidate as a separation medium to discriminate phosphorylated compounds in a liquid chromatography mode. Pure alumina macroporous monolith has been first synthesized from aluminum salt using propylene glycol as a proton scavenger to thrust the solution pH from acidic into neutral conditions. Alumina-based complex oxides such as garnets and spinels can also be prepared in pure phases. Polymerization and phase separation in organic crosslinker system was also controlled to obtain well-defined co-continuous macro-frameworks instead of those composed of aggregated particles. These examples demonstrate the versatility of using phase-separation in gelling systems to obtain well-defined macroporous structures. © 2007 Materials Research Society.

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Elastic aerogels and xerogels synthesized from methyltrimethoxysilane (MTMS) 査読有り

Kanamori K., Nakanishi K., Hanada T.

Materials Research Society Symposium Proceedings   1134 巻   頁： 173 - 178   2008年9月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Materials Research Society Symposium Proceedings  

Transparent organic-inorganic hybrid aerogels and aerogel-like xerogels have been prepared from methyltrimethoxysilane (MTMS) respectively by supercritical drying (SCD) and ambient pressure drying (APD). The new aerogels and xerogels significantly deform without collapsing on uniaxial compression and almost fully relax when unloaded. This elastic behavior, termed as "spring-back", allows APD without noticeable shrinkage and cracking. The flexible network composed of lower cross-linking density (up to three bonds per every silicon atom) compared to silica gels (up to four bonds) and repulsion between hydrophobic methyl groups bonded to every silicon atom largely contributes to the pronounced deformability and relaxing, respectively. Lower surface silanol group density also plays a crucial role for the "spring-back" behavior. © 2009 Materials Research Society.

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Hierarchically porous oxides, hybrids and polymers via sol-gel accompanied by phase separation 査読有り

Nakanishi Kazuki

ORGANIC/INORGANIC HYBRID MATERIALS - 2007   1007 巻   頁： 51 - 62   2008年

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記述言語：英語   掲載種別：研究論文（学術雑誌）  

Web of Science

Living radical polymerization in size-exclusion silica gel column reactors 査読有り

Katsube M., Ouchi M., Ando T., Sawamoto M., Nakanishi K., Ishizuka N.

Polymer Preprints, Japan   55 巻 ( 1 )   2006年10月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Polymer Preprints, Japan  

This work was aimed to development of continuous-flow living radical polymerization in a silica-gel column, "Chromolith", focusing its separation function by combination of surface chemical absorption and size-exclusion via uniquely shaped mesopores, Thus, living radical copolymerization of two monomers with different polarities, methyl methacrylate (MMA) and 2(dimethylamino)ethyl methacrylate (DMAEMA) was performed with a catalyst [2; Ru(Ind)Cl(PPh3)2] coupled with an initiator (1). Copolymers were continuously produced, and molecular weight distributions were narrower than that in the corresponding batch process.

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New macroporous crosslinked polymer gels prepared via living radical polymerization 査読有り

Kanamori K., Nakanishi K., Hanada T.

Materials Research Society Symposium Proceedings   947 巻   頁： 66 - 71   2006年

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Materials Research Society Symposium Proceedings  

Macroporous crosslinked polymer gels have been prepared via TEMPO-mediated living radical polymerization of divinylbenzene (DVB) in a solvent with a counter polymer. Incorporating a counter polymer, poly(dimethylsiloxane) (PDMS), induced macroscopic spinodal-type phase separation during the course of polymerization of DVB while suppressing the segregation of DVB-derived particles from the solution by living polymerization. Well-defined macroporous morphologies comprising continuous DVB-derived skeletons have thus obtained. Macropore volume and diameter were independently controlled by altering the concentrations of PDMS and the solvent. Since the present polymer gels are prepared using only the multifunctional "crosslinker", mechanical durability against bending and compression was found to be as high as inorganic ceramics with similar morphologies and porosities. © 2007 Materials Research Society.

DOI： 10.1557/proc-0947-a03-27

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Monolithic O/I-hybrids with hierarchically ordered meso- And macropores 査読有り

Nakanishi K., Kobayashi Y., Amatani T., Hirao K., Kodaira T.

Materials Research Society Symposium Proceedings   847 巻   頁： 147 - 157   2005年12月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Materials Research Society Symposium Proceedings  

Organic-Inorganic hybrid gels with hierarchical well-defined macropores and supramolecularly templated mesopores with long-range orders have been synthesized in the systems of bridged poly(silsesquioxane) systems. Nonionic surfactants such as poly(ethyleneglycol)-poly(propyleneglycol)- poly(ethyleneglycol) triblock copolymers, EOPOEOs, were found to be effective both in inducing the phase separation to give macroporous morphology and in templating the mesopores with narrow size distribution. The number of methylene units in the bridge, changed from 1 to 6 in the present experiments, affected both the phase separation tendency and template strength. In the system containing 1,2-bis(trimethoxysilyl)ethane, 2D-hexagonal arrangement of mesopores have been prepared in the gel skeleton comprising the well-defined continuous macroporous network with an aid of micelle-stabilizing agent. © 2005 Materials Research Society.

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Hierarchical macro-mesoporous silica monolith 査読有り

Amatani T., Nakanishi K., Hirao K., Kodaira T.

Materials Research Society Symposium Proceedings   847 巻   頁： 121 - 126   2005年12月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Materials Research Society Symposium Proceedings  

Monolithic pure silica gels with hierarchical macro-mesoporous structure have been synthesized via spontaneous sol-gel process from silicon alkoxidc using a structure-directing agent and a micelle-swelling agent. Monolithic body with well-defined co-continuous macropores is a result of concurrent phase separation and sol-gel transition induced by the polymerization reaction, whereas the mesopores are templated by the cooperative self-assembly of inorganic species, a structure-directing agent and a micelle-swelling agent. The following removal of surfactants by heat-treatment gives silica gels with hierarchical and fully accessible pores in discrete size ranges of micrometers and nanometers. The highly ordered 2D-hexagonal arrays of mesopores have been confirmed by X-ray diffraction measurements and FE-SEM observations. Furthermore, by further additions of the micelle-swelling agent, the mesostructural transition from well-ordered 2D-hexagonal arrays to mesostructured cellular foams (MCF) have been induced accompanied by minor modifications of the micrometer-range structure. © 2005 Materials Research Society.

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Living radical polymerization in ruthenium-bearing size-exclusion silica gel column reactors 査読有り

Katsube M., Ando T., Ouchi M., Sawamoto M., Nakanishi K., Ishizuka N.

Polymer Preprints, Japan   54 巻 ( 2 )   2005年12月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Polymer Preprints, Japan  

A catalyst corresponding to Ru(Ind)Cl(PPh3)2 was covalently supported onto a mesopore and silica-gel (Chromolith™) to construct a "size-exclusion column reactor" in which "physical control" of polymer molecular weight is expected by the retention-time difference of each mobile substrate according to its size exclusion (Scheme 2). With Ru(II)-catalyzed living radical polymerization continuously performed in this column, better reaction control is expected by not only the supported catalyst but by this column separation (Fig. 1). The Ru-bearing column 5 (powder form) in fact induced living radical polymerization of methyl methacrylate with initiator 6 and an additive (n-Bu2NH) in toluene at 80°C (Fig. 2). Continuous flow polymerization in the column reactor will be discussed and compared with those in batch systems.

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Mechanical and thermal properties of porous polyimide monoliths crosslinked with aromatic and aliphatic triamines 査読有り

Ishida Mitsuhiro, Sashiyama Yutaro, Akamatsu Hirofumi, Hayashi Katsuro, Nakanishi Kazuki, Hasegawa George

JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY   104 巻 ( 3 ) 頁： 526 - 535   2022年12月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Journal of Sol-Gel Science and Technology  

Thermal insulating materials are of importance for efficient and effective use of heat energy. Porous organic foams are widely employed for this purpose owing to their low thermal conductivity and mass productivity at low cost. However, the poor thermal stability of organic polymers limits their availability within a low temperature range (typically, < 150 °C). In this paper, we demonstrate the one-pot sol–gel synthesis of porous poly(amic acid) (PAA) xerogels and their conversion to porous polyimide (PI) monoliths by thermal imidization. The PAA networks crosslinked with either aromatic or aliphatic triamine and the bicontinuous porous morphology tailored via spinodal decomposition allow the evaporative drying at ambient pressure to obtain low-density PAA xerogels without significant shrinkage. The aromatic crosslinker yields the porous PI monoliths with higher porosity and flexible feature as compared with those prepared with the aliphatic triamine. On the other hand, the porous PI monolith based on the aliphatic crosslinker possesses slightly higher thermal stability owing to the stiffer mechanical property. The durability test results verify the porous PI thermal insulators are available in air at up to ~450 °C for a short period and up to ~350 °C for a long term. [Figure not available: see fulltext.]

DOI： 10.1007/s10971-022-05843-8

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その他リンク： https://link.springer.com/article/10.1007/s10971-022-05843-8/fulltext.html

Dedicated to Professor Sumio Sakka, Founding Editor of Journal of Sol-Gel Science and Technology 査読有り

Nakanishi Kazuki, Kozuka Hiromitsu

JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY   104 巻 ( 3 ) 頁： 447 - 448   2022年12月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Journal of Sol-Gel Science and Technology  

DOI： 10.1007/s10971-022-05955-1

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Amphiphilic Copolymer-Modified Eggshell-Based Column Packing Materials for the Preparative Separation of Basic Drugs 査読有り

Yoshii T., Mochida M., Kaizu K., Soda Y., Kanamori K., Nakanishi K., Sato T., Imai H., Citterio D., Hiruta Y.

ACS Applied Polymer Materials   4 巻 ( 10 ) 頁： 6949 - 6957   2022年10月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：ACS Applied Polymer Materials  

A way to utilize eggshells is desired because most of the eggshell waste is disposed of in landfills. Despite eggshells having attractive features such as a thermodynamically stable porous crystalline structure, their effective utilization as a functional material has yet to be demonstrated. Herein, we developed an alkali-stable column packing material for reversed-phase preparative high-performance liquid chromatography (HPLC) based on eggshells. Nanocrystals and biopolymers present on eggshell powder were removed by surface treatment with buffered ethylenediaminetetraacetic acid (EDTA) and sodium hypochlorite solutions, resulting in bare calcium carbonate with a uniform porous surface. The obtained particles were modified with poly(maleic acid-alt-1-octadecene) (PMAcO) having hydrophobic alkyl chains and anionic carboxylate groups. The prepared PMAcO-modified eggshell-based material was applied to an HPLC column, and its performance is evaluated. The column succeeded in the separation of alkylbenzenes, steroids, and diastereomers. It was also used for the separation of basic tricyclic antidepressants in an alkaline mobile phase, showing excellent retention capacity and alkali stability. This study demonstrates the potential of eggshell utilization, providing not only a practical stationary phase for HPLC but also a solution for recycling calcium carbonate-based biomineral waste.

DOI： 10.1021/acsapm.2c00866

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Oxide-on-Oxide Porous Electrodes Revealing Superior Reversible Li+-Coupled Electron-Transfer Properties by Unconventional Heterojunction Effects 査読有り

Hara Yosuke, Shigetake Rikuo, Nakanishi Kazuki, Kanamori Kazuyoshi, Sakaushi Ken

ACS APPLIED MATERIALS & INTERFACES   14 巻 ( 31 ) 頁： 35883 - 35893   2022年7月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：ACS Applied Materials and Interfaces  

Internal spacing of electrodes is a key point for controlling electron-transfer (ET)-related phenomena. However, their disordered porous structures often prevent the observation of microscopic effects. It hampers the development of modern electrochemical theories. The development of model porous electrodes therefore provides an ideal platform to discover intriguing fundamental principles of electrode processes. We developed a new synthetic strategy for all-oxide monolithic ruthenium dioxide (RuO2)/antimony-doped tin oxide (ATO) electrodes with a controlled hierarchically porous structure and oxide-oxide heterojunction. The use of the obtained RuO2/ATO electrodes as model electrodes suppressed influences related to different mass diffusion efficiencies between electrodes with heterojunctions of different types. Then, we showed unconventional oxide-oxide heterojunction effects, improving reversible Li+-coupled electron-transfer properties using model electrodes constituted of various nanostructured (nano-) RuO2 on porous ATO. In addition to the superior electrochemical properties of the nano-RuO2/ATO heterojunction, the quasi-two-dimensional (2D) RuO2/ATO heterojunction led to improved specific capacity at a high rate and longer cycle life. We anticipate that this oxide-oxide heterojunction effect and developed all-oxide model porous electrodes can provide a path to develop advanced reversible energy storage devices.

DOI： 10.1021/acsami.2c06297

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Porous polymer-derived ceramics: Flexible morphological and compositional controls through sol–gel chemistry 査読有り

Hasegawa G., Kanamori K., Nakanishi K.

Journal of the American Ceramic Society   105 巻 ( 1 ) 頁： 5 - 34   2022年1月

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記述言語：日本語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Journal of the American Ceramic Society  

Porous nonoxide ceramics have exhibited impressive progress in terms of synthesis and applications over the past few decades because of their unique characteristics distinguished from the oxide counterparts. From the synthetic aspect, the preceramic polymer route, where nonoxide ceramics such as carbides and nitrides are produced from molecular precursors, offers exceptional opportunities to elaborate and control the material shape as well as the micro- and nanostructures in concert with various techniques. This review presents monolithic ceramic materials based on various reduced phases bearing hierarchical porosity with a focus on those obtained from macroporous preceramic monoliths prepared via the one-pot sol–gel process accompanied by spinodal decomposition. Here, we highlight two classes of preceramic inorganic–organic hybrid gels: organometallic crosslinked polymers based on poly(silsesquioxane)s and nonorganometallic hybrid networks related to Ti without Ti–C bonds. The polymer-to-ceramic conversion processes are discussed with concern for the crystal transition behaviors and the variation of pore properties in different length scales upon heating. In addition, although out of the preceramic polymer category, some examples of inorganic–organic nanocomposite gels with a carbonizable polymer and/or urea for yielding porous metal carbides and nitrides in a monolithic form are introduced as well, which provides extended versatility toward a variety of transition metal systems.

DOI： 10.1111/jace.18130

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Designing hierarchical porosity in tin oxide monoliths and their application as a solid acid catalyst 査読有り

Suzuki Yoshinao, Hasegawa George, Kanamori Kazuyoshi, Nakanishi Kazuki

NEW JOURNAL OF CHEMISTRY   45 巻 ( 37 ) 頁： 17558 - 17565   2021年10月

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記述言語：英語   掲載種別：研究論文（学術雑誌）   出版者・発行元：New Journal of Chemistry  

Hierarchically porous tin oxide monoliths have been prepared for the first time from a low-cost tin(iv) chloride precursor through an epoxide-mediated sol-gel process in an aprotic solvent N,N-dimethylformamide. Phase separation is induced in the presence of poly(propylene glycol) in the course of polymerization triggered by an acid scavenger, propylene oxide, leading to macroporous tin-based oxyhydroxide monoliths. The resultant macropores are confirmed to be controlled in the size range of 0.9-2.9 μm. Both the post-gelation solvothermal treatment in 2-propanol and calcination in air gave rise to crystallinity and mesoporosity (2.4-103 nm in size with BET surface area up to 261 m2 g-1), and hierarchically porous tin oxide monoliths have been obtained for the first time. The monoliths are demonstrated as a catalyst for the esterification of valeric acid and methanol. This journal is

DOI： 10.1039/d1nj03307g

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Sol-gel based structural designs of macropores and material shapes of metal-organic framework gels 査読有り

Hara Y., Manabe K., Nakanishi K., Kanamori K.

Materials Advances   2 巻 ( 13 ) 頁： 4235 - 4239   2021年7月

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記述言語：日本語   掲載種別：研究論文（学術雑誌）   出版者・発行元：Materials Advances  

We have developed a general synthetic strategy to control macroporous structures and material shapes of metal-organic framework (MOF) gels via a sol-gel based structural control process. A series of 1,3,5-benzene tricarboxylic acid (BTC) based MOF gels, Cr-BTC and Zr-BTC, have been chosen as a proof of concept.

DOI： 10.1039/d0ma01009j

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