Organotemplate-free Synthesis and Proton Conduction Properties of a Layered Aluminophosphate Na4[Al4P4O18]·H2O†

doi:10.7503/cjcu20150685

Abstract

Abstract:

In the organotemplate-free system, a layered aluminophosphate Na₄[Al₄P₄O₁₈]·H₂O(1) was synthesized with Na⁺ ion as the structure-directing agent under hydrothermal condition. The structure was determined by single-crystal X-ray diffraction, and further characterized by powder X-ray diffraction(PXRD), scanning electron microscopy(SEM), inductively coupled plasma(ICP) and thermal gravimetric(TG) analyses. Compound 1 crystallizes in the monoclinic space group P2₁/c with a=1.00887(9) nm, b=0.86747(8) nm, c=0.97580(9) nm, V=0.77387(12) nm³, and Z=2, and its framework consists of AlO₅ and PO₄ units. Compound 1 possesses high thermal stability, and the crystal structure remains unchanged after calcination at 400 ℃ in air. The proton conductivity measurement gives that compound 1 possesses excellent conductivity with σ the value of 1.19×10^-3 S/cm when immersed in water at 55 ℃, which is higher than those of traditional zeolitic materials.

Key words: Zeolite, Layered aluminophosphate, Proton conductivity, Hydrothermal synthesis

CLC Number:

O611.4

TrendMD:

WANG Ning, SUN Qiming, YAN Yan, LIU Jiancong, YU Jihong, XU Ruren. Organotemplate-free Synthesis and Proton Conduction Properties of a Layered Aluminophosphate Na₄[Al₄P₄O₁₈]·H₂O^†[J]. Chem. J. Chinese Universities, 2015, 36(11): 2311.

Figures/Tables 11

References 33

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Empirical formula	Al₄P₄O₁₉H₂Na₄	Calculated density/(Mg·m^-3)	2.694
Crystal system	Monoclinic	Absorption coefficient/mm^-1	0.940
Space group	P2₁/c	F(000)	616
a/nm	1.00887(9)	Limiting indices	-13≤h≤7, -11≤k≤11, -11≤l≤13
b/nm	0.86747(8)	Reflections collected/unique[R(int)=0.0270]	5485/1935
c/nm	0.97580(9)	Refinement method	Full-matrix least-squares on F²
α/(°)	90	Data/restraints/parameters	1935/7/152
β/(°)	115.0160(10)	Goodness-of-fit on F²	1.041
γ/(°)	90	Final R indices[I>2σ(I)]	R₁=0.0307, wR₂=0.0795
V/nm³	0.77387(12)	R indices(all data)	R₁=0.0386, wR₂=0.0835
Z	2

Empirical formula	Al₄P₄O₁₉H₂Na₄	Calculated density/(Mg·m^-3)	2.694
Crystal system	Monoclinic	Absorption coefficient/mm^-1	0.940
Space group	P2₁/c	F(000)	616
a/nm	1.00887(9)	Limiting indices	-13≤h≤7, -11≤k≤11, -11≤l≤13
b/nm	0.86747(8)	Reflections collected/unique[R(int)=0.0270]	5485/1935
c/nm	0.97580(9)	Refinement method	Full-matrix least-squares on F²
α/(°)	90	Data/restraints/parameters	1935/7/152
β/(°)	115.0160(10)	Goodness-of-fit on F²	1.041
γ/(°)	90	Final R indices[I>2σ(I)]	R₁=0.0307, wR₂=0.0795
V/nm³	0.77387(12)	R indices(all data)	R₁=0.0386, wR₂=0.0835
Z	2

Atom	x	y	z	U_eq	Atom	x	y	z	U_eq
Al1	6752(1)	2981(1)	7649(1)	10(1)	O6	7890(2)	-346(2)	10647(2)	21(1)
Al2	3834(1)	3981(1)	4444(1)	10(1)	O7	3461(2)	-542(2)	6108(2)	15(1)
P1	3981(1)	1123(1)	6456(1)	10(1)	O8	5577(2)	4088(2)	6003(2)	12(1)
P2	8624(1)	1262(1)	10900(1)	11(1)	O9	10259(2)	1107(2)	11597(2)	24(1)
O1	3307(2)	2031(2)	4977(2)	14(1)	O1W	-75(17)	220(20)	5430(40)	43(5)
O2	5659(2)	1229(2)	7131(2)	14(1)	O1W'	0	0	5000	43(6)
O3	8109(2)	2037(2)	9368(2)	18(1)	Na1	9545(1)	7345(2)	5822(2)	32(1)
O4	8167(2)	2807(2)	6972(2)	18(1)	Na2	2594(1)	4450(1)	7686(2)	34(1)
O5	3481(2)	1845(2)	7602(2)	14(1)

Atom	x	y	z	U_eq	Atom	x	y	z	U_eq
Al1	6752(1)	2981(1)	7649(1)	10(1)	O6	7890(2)	-346(2)	10647(2)	21(1)
Al2	3834(1)	3981(1)	4444(1)	10(1)	O7	3461(2)	-542(2)	6108(2)	15(1)
P1	3981(1)	1123(1)	6456(1)	10(1)	O8	5577(2)	4088(2)	6003(2)	12(1)
P2	8624(1)	1262(1)	10900(1)	11(1)	O9	10259(2)	1107(2)	11597(2)	24(1)
O1	3307(2)	2031(2)	4977(2)	14(1)	O1W	-75(17)	220(20)	5430(40)	43(5)
O2	5659(2)	1229(2)	7131(2)	14(1)	O1W'	0	0	5000	43(6)
O3	8109(2)	2037(2)	9368(2)	18(1)	Na1	9545(1)	7345(2)	5822(2)	32(1)
O4	8167(2)	2807(2)	6972(2)	18(1)	Na2	2594(1)	4450(1)	7686(2)	34(1)
O5	3481(2)	1845(2)	7602(2)	14(1)

Al1—O4	0.18147(18)	Al2—O1	0.19098(18)	P2—O6	0.15493(19)
Al1—O8	0.18163(18)	Al2—Al2#3	0.27720(14)	O4—P2#2	0.15384(18)
Al1—O2	0.18198(18)	P1—O7	0.15253(17)	O5—Al2#4	0.18248(18)
Al1—O7#1	0.18381(18)	P1—O1	0.15275(17)	O6—Al2#5	0.18002(19)
Al1—O3	0.18482(18)	P1—O2	0.15375(18)	O7—Al1#5	0.18381(18)
Al2—O8	0.17752(18)	P1—O5	0.15413(17)	O8—Al2#3	0.18895(17)
Al2—O6#1	0.18002(19)	P2—O9	0.15006(19)	O1W—O1W'	0.050(4)
Al2—O5#2	0.18248(18)	P2—O3	0.15164(17)	O1W—O1W#6	0.099(9)
Al2—O8#3	0.18895(17)	P2—O4#4	0.15384(18)	O1W'—O1W#6	0.050(4)
O4—Al1—O8	92.40(8)	O6#1—Al2—O1	85.80(8)	O9—P2—O6	110.56(11)
O4—Al1—O2	107.89(9)	O5#2—Al2—O1	87.70(8)	O3—P2—O6	107.49(11)
O8—Al1—O2	95.95(8)	O8#3—Al2—O1	177.59(8)	O4#4—P2—O6	108.68(10)
O8—Al1—O7#1	90.01(8)	O6#1—Al2—Al2#3	117.05(7)	P1—O2—Al1	126.64(10)
O2—Al1—O7#1	122.63(9)	O5#2—Al2—Al2#3	114.53(7)	P2—O3—Al1	154.78(12)
O4—Al1—O3	84.21(8)	O8#3—Al2—Al2#3	39.33(5)	P2#2—O4—Al1	135.39(11)
O8—Al1—O3	173.26(9)	O1—Al2—Al2#3	138.29(7)	P1—O5—Al2#4	124.65(11)
O2—Al1—O3	90.64(8)	O7—P1—O1	107.72(9)	P2—O6—Al2#5	133.37(11)
O7#1—Al1—O3	87.62(8)	O7—P1—O2	111.38(10)	P1—O7—Al1#5	129.71(10)
O8—Al2—O6#1	127.69(9)	O1—P1—O2	110.14(10)	Al2—O8—Al1	140.33(10)
O8—Al2—O5#2	125.03(9)	O7—P1—O5	111.00(10)	Al2—O8—Al2#3	98.24(8)
O6#1—Al2—O5#2	107.27(9)	O1—P1—O5	108.93(10)	Al1—O8—Al2#3	121.43(9)
O8—Al2—O8#3	81.76(8)	O2—P1—O5	107.65(10)	O1W'—O1W—O1W#6	0.002(15)
O6#1—Al2—O8#3	95.32(8)	O9—P2—O3	109.84(11)	O1W—O1W'—O1W#6	180.00(2)
O5#2—Al2—O8#3	94.00(8)	O9—P2—O4#4	109.07(11)
O8—Al2—O1	95.87(8)	O3—P2—O4#4	111.19(10)

Organotemplate-free Synthesis and Proton Conduction Properties of a Layered Aluminophosphate Na₄[Al₄P₄O₁₈]·H₂O^†

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