Method for preparing high-performance Silicalite-1 molecular sieve membrane in super-dilute synthetic fluid

A dilute synthetic liquid and molecular sieve technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of unseen literature reports, synthetic membrane performance reports, and inability to realize industrialization, so as to improve flux and selectivity, content reduction, and preparation cost reduction

Active Publication Date: 2010-02-24
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Many scientific research institutions in my country, such as Tsinghua University, Peking University, Fudan University, Zhejiang University, Nanjing University of Technology, Tianjin University, Dalian University of Technology, etc. agent, or the flux and separation factor of the synthetic membrane are low, and its industrialization cannot be realized
[0006] In the existing reports, the Silicalite-1 molecular sieve membranes investigated by the researchers were prepared at lower H 2 O / SiO 2 Molar ratio of synthetic solution prepared in H 2 O / SiO 2 Sols higher than 300 have not yet reported the performance of synthetic films, while in H 2 O / SiO 2 The synthesis in the sol higher than 500 has not been reported in the literature

Method used

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  • Method for preparing high-performance Silicalite-1 molecular sieve membrane in super-dilute synthetic fluid
  • Method for preparing high-performance Silicalite-1 molecular sieve membrane in super-dilute synthetic fluid
  • Method for preparing high-performance Silicalite-1 molecular sieve membrane in super-dilute synthetic fluid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Synthesis of embodiment 1 Silicalite-1 molecular sieve crystal

[0041] Take a certain amount of TPAOH aqueous solution and flaky NaOH dissolved in deionized water, stir to dissolve and cool to room temperature, then continue to add a certain amount of silica sol to the above solution, and finally the composition (molar ratio) of each component in the solution is SiO 2 : 0.3TPAOH : 0.15NaOH : 45H 2 O, then aging at room temperature, after aging for 24 hours, put it into a stainless steel reactor, and put the stainless steel reactor into an oven at 130°C for 30 hours to synthesize. The synthesized crystals were washed with deionized water until neutral and then dried. After drying, they were placed in a muffle furnace and calcined at 550° C. for 12 hours to remove the template agent (such as figure 1 ). Calcined crystals are detected by XRD (X-ray diffraction) and show to be Silicalite-1 crystals (such as figure 2 ), and the molecular sieve crystals are in the shape ...

Embodiment 2

[0042] Embodiment 2 Preparation of Silicalite-1 molecular sieve membrane

[0043] The carrier used in this experiment is the tubular mullite produced by Japan Nikkato Co., Ltd. (the composition of mullite is 67wt.%Al 2 o 3 and 33wt.% SiO 2 ) as a carrier for synthesizing Silicalite-1 membrane, the inner diameter and outer diameter of the carrier are 9mm and 12mm respectively, the length is 100mm, the porosity is about 43%, and the average pore diameter is about 1 μm. Ultrasonic cleaning in deionized water and drying for later use. The dried carrier is coated with self-made Silicalite-1 molecular sieve.

[0044] Weigh a certain amount of TPAOH and deionized water and stir evenly to make it a uniform solution, then add a certain amount of TEOS to the above solution and continue stirring and aging at room temperature until it becomes a clear and transparent solution at room temperature. The composition (molar ratio) of each component in the solution is TEOS: 0.3TPAOH: 500H 2...

Embodiment 3

[0049] Embodiment 3 Preparation of Silicalite-1 molecular sieve membrane

[0050] The synthetic liquid raw material and operation that adopt are as embodiment 2, just the proportioning of the synthetic liquid that forms is TEOS: 0.3TPAOH: 600H 2 O, other preparation steps are identical with embodiment 2. After calcination, the Silicalite-1 molecular sieve membrane was used for pervaporation experiments and characterizations. The results of the pervaporation experiments are shown in S-3 and S-4 in Table 2.

[0051] Table 2 Pervaporation separation performance of Silicalite-1 molecular sieve membrane on mullite carrier (60℃)

[0052]

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Abstract

The invention relates to a method for preparing a high-performance Silicalite-1 molecular sieve membrane in super-dilute synthetic fluid, comprising the following steps: using low-cost silica solutionas a synthesis material to prepare a Silicalite-1 molecular sieve crystal with high activity, using the Silicalite-1 molecular sieve crystal as a seed crystal and loading the seed crystal on the surface of a support body, and preparing the high-performance Silicalite-1 molecular sieve membrane on a mullite support body using super- diliute synthetic fluid (H2O / SiO2=200-200). The invention not only effectively improves the performance of the Silicalite-1 molecular sieve membrane, but also greatly reduces the requirement of silicon source and template agent in the membrane synthetic fluid and greatly reduces the preparation cost of membrane. The membrane can be widely used for occasions of high-temperature fluid separation, gas separation, membrane reactors, and the like. The invention remarkable improves the flux penetration and the selectivity of the Silicalite-1 molecular sieve membrane, reduces the production cost and is suitable for industrial production.

Description

technical field [0001] The invention provides a kind of self-made highly active Silicalite-1 molecular sieve as crystal seed, adopts ultra-dilute synthetic liquid (H 2 O / SiO 2 =500-2000), a method for rapidly forming a layer of Silicalite-1 molecular sieve crystals on the outer surface of the porous mullite tube. It belongs to the field of permeation separation of inorganic materials. Background technique [0002] In recent years, the research on the preparation and application of molecular sieve membranes has received extensive attention. Zeolite membranes can not only be used for the dehydration of organic solvents, but also show good separation performance in the recovery of low-concentration organics in aqueous solutions. Compared with organic membranes, molecular sieve membranes not only have many advantages such as high temperature resistance, good chemical stability, and high mechanical strength, but also have good separation selectivity and large permeation. resea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D69/10
Inventor 陈祥树周荣飞朱美华
Owner JIANGXI NORMAL UNIV
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