Synthesis and Characterization of Highly Stable Nano-Sized Y Zeolite

doi:10.19894/j.issn.1000-0518.250291

Chinese Journal of Applied Chemistry ›› 2026, Vol. 43 ›› Issue (3): 373-386.DOI: 10.19894/j.issn.1000-0518.250291

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Synthesis and Characterization of Highly Stable Nano-Sized Y Zeolite

Jing-Hang XUE(), Bo QIN, Wei LIU, Tong ZHANG, Wen-Jie XIE

Sinopec Dalian Research Institute of Petroleum and Petrochemicals，Dalian 116045，China

Received:2025-07-20 Accepted:2025-10-16 Published:2026-03-01 Online:2026-03-26
Contact: Jing-Hang XUE
About author:xuejinghang.fshy@sinopec.com
Supported by:
the Joint Funds of the National Natural Science Foundation of China(U24A202895)

Abstract

Abstract:

Nano-sized Y zeolite has attracted increasing attention in the petroleum refining industry due to its excellent diffusion properties and abundant external surface acid sites. However， synthesizing highly stable nanosized Y zeolite still remains challenging. A novel hydrothermal crystallization method was developed using inexpensive anionic surfactant ammonium fatty alcohol ether sulfate （AESA） as a template agent. The synthesis involved a strategy of multiple gel formation steps， multi-stage crystallization， and post-addition of silicon source. The effects of synthesis conditions， AESA/Al₂O₃ ratio， and Na₂O/Al₂O₃ ratio on the morphology and physicochemical properties of the zeolite were investigated. The synthesized materials were characterized by powder X-ray diffraction （XRD）， X-ray fluorescence spectroscopy （XRF）， N? physisorption fourier transform infrared spectroscopy （FT-IR）， pyridine-adsorbed FT-IR （Py-FTIR）， solid-state NMR （²⁹Si MAS NMR and ²⁷Al MAS NMR）， scanning electron microscopy （SEM）， transmission electron microscopy （TEM）， and EDS-mapping. The hydrothermal stability at high temperatures was compared between the nano-sized Y and commercial Y zeolites. The results demonstrate that under optimized synthesis conditions， the nano-sized zeolite exhibits an average particle size of 83 nm， a silica-alumina ratio （SAR） of 5.8， a unit cell parameter of 24.62 ?， and a specific surface area of 887 m2/g. After hydrothermal treatment at 600 °C， the reduction rate of relative crystallinity was 16.0%， which recovered to 7.1% after acid treatment. Compared to commercial Y zeolite， the nano-sized Y zeolite possesses highly developed secondary pore structure （pore size distribution mainly in the 10~80 nm range）， retains more acid sites， and exhibits superior stability， which were attributed to its improved framework integrity and higher SAR.

Key words: Y zeolite, Nano-sized, High stability

CLC Number:

O611.4

Jing-Hang XUE, Bo QIN, Wei LIU, Tong ZHANG, Wen-Jie XIE. Synthesis and Characterization of Highly Stable Nano-Sized Y Zeolite[J]. Chinese Journal of Applied Chemistry, 2026, 43(3): 373-386.

Figures/Tables 21

Fig.1 Synthesis strategies for highly stable nano-sized Y zeolite

Fig.2 XRD spectra of products obtained by different synthesis methods

Table 1 Physicochemical properties of products obtained by different synthesis methods

Sample	S_BET/（m²·g^-1）	V_total/（cm³·g^-1）	SAR
Nanoy-b	858	0.37	5.3
Nanoy-c	861	0.40	5.1
Nanoy-d	856	0.37	4.9
Nanoy-e	859	0.40	4.6

Fig.3 SEM images of products obtained by different synthesis methods

Fig.4 XRD patterns of products synthesized with different n（AESA）/n（Al2O3）

Fig.5 FT-IR spectra of products synthesized with different n（AESA）/n（Al2O3）

Fig.6 （A） N2 adsorption-desorption isotherms and （B） pore size distributions of samples with different n（AESA）/n（Al2O3）

Fig.7 2?Si （A， B， C， D， E） and 2?Al （F） MAS NMR spectra of products synthesized with different n（AESA）/n（Al2O3）

Table 2 The SAR of products with different n（AESA）∶n（Al2O3）

Sample	SAR （XRF）	a₀/?	SAR （XRD） ^a	Composition/% of Q⁴（nAl）				SAR （²⁹Si NMR） ^b
Sample	SAR （XRF）	a₀/?	SAR （XRD） ^a	3	2	1	0	SAR （²⁹Si NMR） ^b
Nanoy-13.3-0.1	5.2	24.64	5.4	13.4	35.2	43.6	7.8	5.2
Nanoy-13.3-0.3	5.3	24.64	5.4	12.5	33.9	44.9	8.7	5.3
Nanoy-13.3-0.7	5.4	24.63	5.6	14.5	30.5	45.9	9.1	5.3
Nanoy-13.3-1.5	5.7	24.60	6.1	9.8	33.0	46.7	10.5	5.6
Nanoy-13.3-2.2	5.7	24.60	6.1	9.0	32.5	48.0	10.5	5.7
Nanoy-13.3-3.0	5.9	24.61	6.0	-	-	-	-	-

Fig.8 SEM images of synthesized products with different n（AESA）/n（Al2O3）

Fig.9 TEM images of synthesized products with different n（AESA）/n（Al2O3）

Fig.10 XRD patterns of synthesized products with different n（Na2O）/n（Al2O3）

Table 3 Physicochemical properties of synthesized products with different n（Na2O）∶n（Al2O3）

Sample	S_BET/（m²·g^-1）	S_micro/（m²·g^-1）	S_meso/（m²·g^-1）	V_total/（cm³·g^-1）	V_micro/（cm³·g^-1）	V_meso/（cm³·g^-1）	SAR	a₀/?	Relative crystallinity/%
Nanoy-12.3-0.5	832	764	68	0.38	0.30	0.08	6.0	24.61	77.77
Nanoy-12.8-0.5	874	799	75	0.40	0.32	0.08	6.0	24.61	75.21
Nanoy-13.3-0.5	865	790	75	0.40	0.32	0.08	5.6	24.63	64.07
Nanoy-13.8-0.5	859	783	76	0.40	0.31	0.09	5.4	24.64	65.49
Nanoy-14.3-0.5	844	767	77	0.39	0.31	0.08	4.2	24.73	64.24
Nanoy-14.8-0.5	651	597	54	0.33	0.24	0.09	4.1	24.74	47.08

Fig.11 SEM images of synthesized products with different n（Na2O）/n（Al2O3）

Fig.12 TEM images of nano-sized Y zeolite under different scales：（A） 500 nm （inset： particle size distribution from TEM）；（B） 100 nm

Fig.13 TEM-EDS elemental mapping images of nano-sized Y zeolite

Fig.14 XRD patterns of Y zeolite：（A） After ammonium ion exchange；（B） After high-temperature（600 ℃） hydrothermal treatment；（C） After acid treatment

Table 4 Comparison of the physicochemical properties of commercial Y and nanosized Y zeolite

Sample	S_BET/（m²·g^-1）	S_micro/（m²·g^-1）	S_meso/（m²·g^-1）	V_total/（cm³·g^-1）	V_micro/（cm³·g^-1）	V_meso/（cm³·g^-1）	SAR	a₀/?	Relative crystallinity/%	Reduction rate of relative crystallinity ^x /%
Coml Y	850	797	53	0.36	0.32	0.04	5.0	24.67	93.0	-
Nano Y	887	807	80	0.41	0.32	0.09	5.8	24.62	73.0	-
Coml-USY	537	431	106	0.33	0.17	0.16	5.0	24.39	51.2	44.9
Nano-USY	623	549	74	0.36	0.22	0.14	5.8	24.39	61.3	16.0
Coml-AUSY	730	579	151	0.45	0.23	0.22	14.7	24.39	54.9	41.0
Nano-AUSY	786	671	115	0.44	0.27	0.17	15.6	24.38	67.8	7.1

Fig.15 BJH pore diameter distribution of Y zeolite after （A） hydrothermal treatment and （B） acid treatment

Fig.16 Py-FT-IR spectra of Y zeolite after acid treatment （A） Coml-AUSY and （B） Nano-AUSY

Table 5 Py-FT-IR acid content of Y zeolite after acid treatment

Sample	Acid amount（160 ℃）/（mmol·g^-1）				Acid amount（450 ℃）/（mmol·g^-1）
Sample	B	L	B+L	B/L	B	L	B+L	B/L
Coml-AUSY	0.52	0.24	0.76	2.17	0.29	0.07	0.36	4.14
Nano-AUSY	0.61	0.26	0.87	2.35	0.37	0.06	0.43	6.17

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Synthesis and Characterization of Highly Stable Nano-Sized Y Zeolite

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