Synthesis of a hierarchically porous niobium phosphate monolith by a sol–gel method for fructose dehydration to 5-hydroxymethylfurfural,Catalysis Science & Technology

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Synthesis of a hierarchically porous niobium phosphate monolith by a sol–gel method for fructose dehydration to 5-hydroxymethylfurfural
Catalysis Science & Technology ( IF 4.4 ) Pub Date : 2018-06-18 00:00:00 , DOI: 10.1039/c8cy00803e
Da-Ming Gao _{1,

2,

3,

4} , Bohan Zhao _{4,

5,

6,

7,

8} , Haichao Liu _{4,

5,

6,

7,

8} , Kei Morisato _{9,

10,

11,

12,

13} , Kazuyoshi Kanamori _{9,

10,

11,

12,

13} , Zhiyong He _{1,

2,

3,

4} , Maomao Zeng _{1,

2,

3,

4} , Huaping Wu _{4,

14,

15,

16,

17} , Jie Chen _{1,

2,

3,

4} , Kazuki Nakanishi _{9,

10,

11,

12,

13}

Affiliation

State Key Laboratory of Food Science and Technology
Jiangnan University
Wuxi 214122
China
Beijing National Laboratory for Molecular Science
College of Chemistry and Molecular Engineering
Peking University
Beijing 100871
Department of Chemistry
Graduate School of Science
Kyoto University
Kyoto 606-8502
Japan
Key Laboratory of Special Purpose Equipment and Advanced Manufacturing Technology
Zhejiang University of Technology
Ministry of Education and Zhejiang Province
Hangzhou 310014

Hierarchically porous niobium phosphate (NbP) was synthesised via a sol–gel method accompanied by phase separation and employed as a catalyst for fructose dehydration. The niobium precursor was prepared by digesting ammonium niobate(V) oxalate in aqueous H₂O₂ with citric acid as a chelating agent to prevent the precipitation of niobium hydroxide. Poly(acrylamide) and poly(ethylene glycol) were used as phase separation inducers to produce co-continuous macropores and gel skeletons. The NbP sample calcined at 600 °C for 8 h had a high surface area (S_BET ∼140 m² g⁻¹) and large acidity (0.84 mmol-NH₃ g⁻¹). The NbP monolith was amorphous after calcination at 600 °C and transformed into an α-NbOPO₄ phase at 1000 °C. The NbP monolith calcined at 600 °C was an efficient acid catalyst for the dehydration of fructose to 5-hydroxymethylfurfural in water (70% yield) or in aqueous dimethyl sulfoxide (90% yield). The productivity of HMF reached 7.3 × 10⁻² mol h⁻¹ per kg-solution at an initial fructose concentration of 10.0 wt% in water with a catalyst loading of 2.0 wt%.

中文翻译：

溶胶-凝胶法将果糖脱水成5-羟甲基糠醛，合成分级多孔磷酸铌整体

分层多孔的磷酸铌（NbP）是通过溶胶-凝胶法合成的，并进行相分离，并用作果糖脱水的催化剂。通过用柠檬酸作为螯合剂在H ₂ O ₂水溶液中消化铌酸草酸铵（V）草酸盐来制备铌前体，以防止氢氧化铌沉淀。聚丙烯酰胺和聚乙二醇用作相分离诱导剂以产生共连续的大孔和凝胶骨架。在600°C下煅烧8 h的NbP样品具有较高的表面积（S _BET〜140 m ² g ^-1）和较大的酸度（0.84 mmol-NH ₃ g ^-1））。NBP的整料在600℃煅烧后的无定形并转化成α-NbOPO ₄相在1000℃。在600°C下煅烧的NbP整体料是一种有效的酸催化剂，可用于将果糖在水（70％的收率）或二甲基亚砜水溶液（90％的收率）中脱水成5-羟甲基糠醛。在水中果糖初始浓度为10.0 wt％，催化剂负载为2.0 wt％的情况下，HMF的生产率达到每千克溶液7.3×10 ^-2 mol h ^-1。

更新日期：2018-06-18

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