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A Simple Preparation Method of Continuous Dense Mordenite Membrane

A mordenite and dense technology, which is applied in the field of inorganic membrane pervaporation separation, can solve the problems of poor binding force between the carrier and the seed crystal, and the inability to prepare zeolite membranes, so as to improve the binding force, good separation performance and repeatability, and improve dispersion sexual effect

Active Publication Date: 2022-03-25
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the current problem that a complete and defect-free zeolite membrane cannot be produced due to the poor binding force between the carrier and the seed crystal, the present invention provides a method for preparing a continuous dense mordenite membrane, by introducing silica-zirconia sol, increasing the number of seeds The OH group in the solution enhances the binding force between the carrier and the seed crystal, improves the dispersion of the seed crystal in the solution, obtains a uniform and continuous seed crystal layer, and prepares a continuous and dense mordenite membrane, which makes the separation effect of the membrane and throughput is significantly increased

Method used

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  • A Simple Preparation Method of Continuous Dense Mordenite Membrane
  • A Simple Preparation Method of Continuous Dense Mordenite Membrane
  • A Simple Preparation Method of Continuous Dense Mordenite Membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0021] (1) Use 600 and 1200 mesh sandpaper to clean the carrier tube (macroporous α-Al 2 o 3 carrier tube) to reduce the surface roughness. After grinding, boil in deionized water for 15 minutes, take it out and let it cool naturally, then put it in an ultrasonic cleaner for 5 minutes to remove residues in the film. After washing with deionized water, both ends are sealed in the Preheat in a blast oven at 175°C for 2 hours.

[0022] (2) Ultrasonic dispersion of mordenite molecular sieve (purchased by Zhonghe Petrochemical, conventional) in 0.5wt.% silica-zirconia sol (Si / Zr=1 in the sol), the concentration of the seed liquid is 3wt.%, Coat the crystal on the carrier tube in step (1) by dipping and pulling method, the soaking time is 25s, take it out and put it into a blast oven to dry at 80°C for 3h.

[0023] (3) Wipe off excess loose seed crystals on the carrier tube in step (2) with absorbent cotton, put it into a control furnace and bake at 550° C. for 6 hours to form a s...

Embodiment 2

[0028] The 0.5 wt.% silica-zirconia sol in step (2) of Example 1 was replaced with 1 wt.% silica-zirconia sol, and the rest of the operations were the same as in Example 1. The pervaporation performance of the prepared mordenite membrane is shown in Table 2.

Embodiment 3

[0030] The 0.5wt.% silica-zirconia sol in step (2) of Example 1 was replaced with 2wt.% silica-zirconia sol, and the rest of the operations were the same as in Example 1. The pervaporation performance of the prepared mordenite membrane is shown in Table 2.

[0031] image 3 It is the particle size distribution figure of silica-zirconia sol in embodiment 1 and embodiment 2-3, as can be seen from the figure that SiO 2 -ZrO 2 The particle size of the sol is about 40nm.

[0032] Figure 4 It is silica-zirconia (a), seed crystal (b) and SiO in embodiment 1 2 -ZrO 2 / The FT-IR spectrogram of seed crystal (c), as can be seen from the figure 3448cm -1 、1636cm -1 and 1400cm -1 The absorption peak at is caused by the stretching vibration, deformation vibration and out-of-plane bending vibration of OH group. Add SiO to the seed 2 -ZrO 2 After sol, 3448cm -1 and 1400cm -1 The peak intensity at , which means that SiO 2 -ZrO 2 The sol increases the OH groups in the seed liqui...

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Abstract

The invention provides a simple preparation method of a continuous and dense mordenite membrane, which mainly solves the problems of poor bonding force between a carrier and a seed crystal layer and the inability to obtain a uniform, complete and high-flux membrane due to the thickness of the seed crystal layer. First, tetraethoxysilane and zirconium n-butoxide were hydrolyzed and copolymerized to prepare polyhydroxyl-containing nano-sized SiO 2 -ZrO 2 sol; disperse micron-sized mordenite (MOR) molecular sieves in silicon-zirconium sol to form a seed liquid; finally, use the dipping and pulling method to coat the seed crystal on the alumina carrier tube, and obtain a complete and continuous seed crystal tube after drying and roasting , and then the second hydrothermal method to grow into a film. The invention effectively solves the problems of defects caused by poor bonding force between the carrier and the seed crystal layer and decrease of membrane flux caused by too thick seed crystal layer.

Description

technical field [0001] The invention belongs to the technical field of inorganic membrane pervaporation separation, relates to a simple preparation method of a continuous dense mordenite membrane, in particular to a method of introducing silica-zirconia sol into a mordenite molecular sieve, which enhances the combination of a carrier and a seed crystal The force improves the dispersibility of the seed crystal, thereby obtaining the preparation method of a complete continuous seed crystal layer. Background technique [0002] Mordenite membrane has good chemical stability and high mechanical strength, and is an excellent acid-resistant material. The higher the silicon-aluminum ratio of the zeolite membrane, the better the acid resistance, and the pervaporation separation in acidic solution shows better stability. At present, most mordenite membranes are synthesized by the secondary growth method. Firstly, the seed crystals are pre-coated on the carrier, and then the complete ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D67/00B01D71/02B01D69/02B01D53/22C07C51/42C07C53/08
Inventor 任秀秀姚政丁明于欢钟璟徐荣
Owner CHANGZHOU UNIV
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