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Progress in Chemistry 2020, Vol. 32 Issue (7): 873-881 DOI: 10.7536/PC190928 Previous Articles   Next Articles

• Review •

Continuous Flow Synthesis of Zeolites

Di Pan1, Peng Liu1, Hongbin Zhang2, Yi Tang1,**()   

  1. 1. Department of Chemistry, Fudan University, Shanghai 200433, China
    2. Preservation and Conservation of Chinese Ancient Books, Fudan University, Shanghai 200433, China
  • Received: Online: Published:
  • Contact: Yi Tang
  • About author:
    ** e-mail:
  • Supported by:
    National Major Research and Development Plan(2018YFA0209402)
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Due to the wide applications of zeolites in various fields, efficient and reliable synthesis of zeolite has become an important research issue. Compared with traditional high-pressure hydrothermal batch synthesis, continuous flow synthesis is one of the new methods for fast preparation of zeolite owing to its short crystallization time and high space-time yield. The high crystalline zeolites can be harvested in minute- and even second-level thanks to the specific characteristics of continuous flow reactors(CFR), such as low thermal lag, controllable mass transfer and good expansibility, which significantly enhance the synthesis efficiency and controllability. In this paper, based on the recent progress, the component of CFR equipment, the advantages and limitations of CFR for zeolite synthesis, and the future applications are introduced and prospected.

Contents

1 Introduction

2 Structure of CFR equipment

2.1 Feeding unit

2.2 Fluid channel

2.3 Heating unit

2.4 Cooling unit

2.5 Back pressure regulator

2.6 Monitor system

3 Features of synthesis process and product

3.1 Features of CFR reaction

3.2 The effective control of crystallization process

3.3 New progress of CFR techniques

4 Limitation of CFR application

4.1 Viscosity

4.2 Blockage

4.3 Crystal aggregation

5 Conclusion and prospect

Key words: continuous flow reactors, thermal lag, zeolite synthesis
Fig.1 The scheme of CFR system for zeolite synthesis
Fig.2 (a) Scheme of the ultrafast CFR synthesis system of ZSM-5,(b) the system temperature changing with time and(c) the system pressure changing with time[32]. Copyright 2016, PNAS
Fig.3 (a) The temperature at different positions in autoclaves changing with time and(b) the system temperature in CFR changing with time through external heating method[37]. Copyright 2016, Elsevier
Table 1 The crystallization time of zeolites and the corresponding conditions in CFR systems
Zeolite type Aging time
(h)		 Aging temperature
(℃)		 Crystallization temperature
(℃)		 Seeding Crystallization time
(min)		 ref
NaA
 50 25 90 NO 13.3 27
\ \ 150 NO 16 36
\ \ 80 NO 20 29
AlPO4-5 24 25 190 YES 1 32
\ \ 160 NO 160 40
SPAO-5 24 90 210 YES 5 33
SPAO-34 24 90 210 YES 10 33
SSZ-13 \ \ 210 YES 10 34
MTN \ \ 210 NO 10 34
ERI \ \ 210 YES 120 38
MOR 0.5 25 260 YES 10 37
ZSM-5 16 90 NO 0.167 31
s-1 \ \ YES 10 48
Fig.4 (a) The29Si MASNMR spectrogram of ERI zeolite synthesized by batch and CFR[39] and(b) the N2 adsorption-desorption curve of ZSM-5 zeolites synthesized by batch and CFR[32]. Copyright 2016, PNAS
Fig.5 NaA zeolites with different diameter distribution synthesized from(a) microchannel CFR and(d) autoclave[28]. Copyright 2006, Elsevier
Fig.6 The theoretical crystallization rate curve of NaA calculated by Arrhenius equation[37]. Copyright 2016, Elsevier
Fig.7 The XRD spectrogram of ZSM-5 product at different time during the ultrafast synthesis at high temperature of(a) 260 ℃ and (b) 300 ℃[32]. Copyright 2016, PNAS
Fig.8 The channel blocked by the aggregation of zeolite crystals[31]. Copyright 2013, Elsevier
Fig.9 The TEM image of(a)ZSM-5[32] and(d)ERI[39]zeolite form CFR synthesis and TEM image of(b)ZSM-5 and(c)ERI zeolite from batch synthesis. Copyright 2016, PNAS
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Abstract

Continuous Flow Synthesis of Zeolites