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Preparation method and application of hierarchical porous molecular sieve membrane

A molecular sieve and channel technology, applied in the field of inorganic membrane preparation, can solve the problems of limiting the development of molecular sieve membranes, high operating pressure, low flux, etc., achieve broad industrial production prospects, reduce energy consumption, and simplify the preparation

Active Publication Date: 2017-02-08
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, due to the small pore size (0.3 nm ~ 1 nm) and compactness of the molecular sieve membrane, the existing molecular sieve membrane only uses its own microporous structure for separation and purification, and water treatment is also limited to the reverse osmosis process. In 2004, Dong et al. For the first time, the MFI molecular sieve membrane was applied to the water-salt reverse osmosis separation system (J. Membr. Sci., 2004(243): 401-404.), the high operating pressure and extremely low flux limit the molecular sieve Development of Membranes in the Field of Water Treatment

Method used

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  • Preparation method and application of hierarchical porous molecular sieve membrane
  • Preparation method and application of hierarchical porous molecular sieve membrane
  • Preparation method and application of hierarchical porous molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0032] Embodiment 1-4 is the preparation of multi-level porous ZSM-5 (MFI type) molecular sieve membrane, the specific experimental steps are as follows:

[0033] (1) Preparation of seed crystals:

[0034] SiO2, tetrapropylammonium hydride, sodium hydroxide and water in molar ratio to SiO 2 :TPAOH:NaOH:H 2 O=1: 0.1~0.5: 0.05~0.2: 5~23 Mix evenly, hydrothermally synthesize at 50°C~180°C for 3 h~15 d, and obtain Silicalite-1 molecular sieves with particle sizes ranging from 50 nm to 500 nm Particles are washed with deionized water until neutral, and then water is added to form a seed crystal suspension with a certain concentration.

[0035] (2) Seed coating:

[0036] Dilute the seed crystal suspension with hydroxypropyl cellulose (HPC) and deionized water to form a seed liquid with a seed crystal mass content of 0.5-5 %, adjust the pH to 3-4 by adding dilute nitric acid, and ultrasonically disperse the seed crystals liquid. A continuous and dense seed crystal layer is coate...

Embodiment 1

[0040] The aforementioned method was used to prepare a hierarchically porous ZSM-5 (MFI type) molecular sieve membrane, as follows:

[0041] (1) Prepare Silicalite-1 seed crystals and configure the molar composition as SiO 2 :TPAOH:NaOH:H 2 O=1:0.3:0.1:14 synthesis solution, pour the synthesis solution into the polytetrafluoroethylene lining of the stainless steel synthesis kettle, hydrothermally synthesize at 60°C for 14 days, the particle size of the prepared Silicalite-1 molecular sieve is about 70 nm, washed with deionized water several times until the pH value of the dispersion tends to be neutral, and then the obtained seeds are dispersed in deionized water to prepare a 10% w.t. seed dispersion.

[0042] (2) The support is coated with seed crystals (such as figure 1 ), mix 10% w.t. seed crystal dispersion with ionized water, dilute nitric acid and hydroxypropyl cellulose, configure 1% w.t. seed crystal liquid, and stir at room temperature for 4 h. A laboratory-made fo...

Embodiment 2

[0045] The preparation process is as shown in Example 1, the difference is that the synthesis conditions of the seed crystals are changed, hydrothermal synthesis is carried out at 120°C for 12 h, and the Silicalite-1 seed crystals with a particle size of about 400 nm are prepared, and other membrane synthesis conditions are the same as in Example 1. , the X-ray diffraction pattern of the film surface is as follows figure 2 Shown in S2.

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Abstract

The invention relates to a preparation method and application of a hierarchical porous molecular sieve membrane. A mesoporous structure guiding agent is added to limit the growth of a molecular sieve crystal, and is subjected to self-assembly in a crystallization process of the molecular sieve crystal, so as to generate a mesoporous structure. The hierarchical porous molecular sieve membrane is synthesized by using a seed crystal inducing secondary nucleation mechanism and a hydrothermal one-step synthesis method; synthesis conditions are mild and controllable, the simplicity in preparation and good repeatability are realized, energy consumption is reduced, and the cost is reduced. The hierarchical porous molecular sieve membrane prepared by adopting the method shows good retention performance, and the retention molecular weight is controllable between 200 and 500000 Da. The method for preparing the hierarchical porous molecular sieve membrane, provided by the invention, can be used for synthesizing the hierarchical porous molecular sieve membrane with other micropore skeleton structures, and has high cost performance and a broad industrial production prospect; the application of the preparation method also can be popularized to the field of catalysis.

Description

technical field [0001] The invention belongs to the field of inorganic membrane preparation, and relates to a preparation method of a multi-stage pore molecular sieve film, in particular to a preparation method of a mesoporous multi-stage pore molecular sieve film and its application in water treatment. Background technique [0002] Membrane separation technology has become one of the important technologies to solve key problems such as energy, food, environment and water resources in the world because of its high efficiency, energy saving and environmental friendliness, and it has attracted more and more attention. According to the classification of membrane properties, membrane materials can be mainly divided into organic membranes, inorganic membranes and liquid membranes. [0003] At present, organic membranes are dominant in industrial ultrafiltration or nanofiltration membranes. The preparation process is simple and the cost is low, but the mechanical strength, anti-po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D71/02B01D69/08C01B39/40
CPCB01D69/08C01B39/40C01P2004/03C01P2002/72B01D2325/0283B01D71/0281B01D67/0049B01D67/0051B01D69/02B01D2323/24B01D2323/12B01D2325/20C01B39/24C01B39/265C01B39/54B01D2323/218B01D2323/21828B01D2325/02831B01D2325/02832B01D67/0067B01D69/081C01P2004/61C02F1/44
Inventor 顾学红姚迅彭莉
Owner NANJING TECH UNIV
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