Synthesis of aluminophosphate xerogels by non-hydrolytic sol-gel condensation of EtAlCl2 with trialkylphosphates

被引:1
|
作者
Podhorsky, Jan [1 ]
Chyba, Jan [1 ]
Pinkas, Jiri [1 ,2 ]
Moravec, Zdenek [1 ,2 ]
机构
[1] Masaryk Univ, Fac Sci, Dept Chem, Kotlarska 267-2, CS-61137 Brno, Czech Republic
[2] Masaryk Univ, CEITEC MU, Kamenice 735-5, Brno 62500, Czech Republic
关键词
Mesoporous xerogels; Aluminium phosphate; Non-hydrolytic synthesis; Sol-gel processing; Alkylhalide elimination mechanism; MOLECULAR-SIEVES; ALUMINUM; CATALYSTS; SURFACE; DEHYDRATION; ADSORPTION; PHOSPHATE; HYDROGEN; METHANOL; ALPO4-21;
D O I
10.1007/s10971-019-04953-0
中图分类号
TQ174 [陶瓷工业]; TB3 [工程材料学];
学科分类号
0805 ; 080502 ;
摘要
We have investigated the preparation of high-surface-area mesoporous aluminophosphates by non-hydrolytic sol-gel method based on reactions of EtAlCl2 with trialkylesters of phosphoric acid (OP(OR)(3), R=Me, Et, Pr-i, Bu-n, in dry organic solvents. The condensations proceed by alkylchloride elimination. Various reaction and calcination conditions were examined. Porosity is obtained after calcination by removal of organic residual groups. This thermal processing at 300 degrees C of as-synthesized precursor gels leads to amorphous aluminophosphate xerogels with surface areas of 400-500m(2)g(-1) provided by small mesopores (2-8nm). Changes in the coordination environment of aluminium from six- to four-coordinate are evidenced by shift of Al-27 MAS NMR resonances. [GRAPHICS] . HighlightsDichloroethylalane reacts with trialkylphosphates by alkylchloride elimination.Aluminophosphate gels are obtained from the non-hydrolytic sol-gel technique.Thermal processing at 300 degrees C leads to amorphous xerogels with surface areas of 400-500m(2)g(-1).Porosity is composed of small mesopores (2-8nm).Templating with Pluronic P123 significantly improves pore size distribution.
引用
收藏
页码:385 / 398
页数:14
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