Method for synthesizing molecular sieve film using vacuum crystal method

A technology of molecular sieve and crystal coating, which is applied in the field of synthesis of molecular sieve membranes, can solve the problems of being unsuitable for industrial amplification, unsuitable for industrial amplification, and difficult to control, and achieves high industrial application value, suitable for industrial amplification, and saving time for coating crystals.

Inactive Publication Date: 2004-12-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Dip-coating method is currently the most commonly used crystal-coating method, but in the process of dip-coating, the molecular sieve seed crystal sol-gel is difficult to be closely combined with the surface of the basement membrane and is easy to flow, so it is difficult to form uniform and continuous crystals. film
The wiping and coating crystal method is the easiest to operate, but it is actually difficult to introduce a uniform and continuous layer of seed crystals on the surface of the base film.
Although the spray coating method can introduce a uniform and continuous seed crystal film on the surface of the flat base film, it is difficult to form a uniform and continuous seed crystal film on the surface of the tubular base film, so it is not suitable for industrial scale-up and has no industrial application value.
Although the laser pulse deposition coating method can introduce a uniform and continuous seed crystal film on the surface of the base film, it requires expensive lasers, so it has no industrial application value
And by adjusting Al 2 o 3 base film and SiO 2 The zata potential of the seed crystal or the method of introducing the seed crystal film on the surface of the base film through electrostatic interaction is complicated to operate, difficult to control, and not suitable for industrial scale-up
These reasons restrict the synthesis of molecular sieve membranes to a certain extent, thus also restricting the industrial application of molecular sieve membranes

Method used

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  • Method for synthesizing molecular sieve film using vacuum crystal method
  • Method for synthesizing molecular sieve film using vacuum crystal method
  • Method for synthesizing molecular sieve film using vacuum crystal method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Step 1 Preparation of seeded base film

[0027] Weigh 1.0 g of type A molecular sieve seed crystals, add 300 ml of distilled water, stir and fully oscillate and disperse in ultrasonic waves, and then fully oscillate and disperse in ultrasonic waves to form a uniform molecular sieve seed crystal suspension 1. The pressure difference between the inner and outer sides of the base film 2 is adjusted to 0.0050MPa by the water pump 3, and the tubular α-Al 2 o 3 The base film was vacuum dip-coated in the prepared molecular sieve seed crystal suspension for 120s and then taken out. After drying, dry and solidify at a certain temperature to obtain a seeded base film.

[0028] Synthesis of Step 2 Type A Zeolite Membrane

[0029] Weigh 156 grams of sodium hydroxide and dissolve in 300 milliliters of distilled water, add 2.1 grams of aluminum foil after clarification, stir to form an aluminum solution; measure 43.5 milliliters of silica sol (SiO 2 27wt%, ρ=1.16g / l) into 390 ml...

Embodiment

[0039] Example Seeded base film Film thickness Total flux Separation coefficient

[0040] Mass (μm) (Kg / m 2 h) (α) (water / isopropanol)

[0041] 1 Uniform and continuous 9 1.72 Above 10000

[0042] 2 Uniform and continuous 14 1.14 5000

[0043] 3 Uniform and continuous 10 1.47 Above 10000

[0044] Synthesis Example 4 of Tubular Type A Molecular Sieve Membrane

[0045] Step 1 Preparation of seeded base film

[0046] Weigh 1.0 g of type A molecular sieve seed crystals, add 300 ml of distilled water, stir and fully oscillate and disperse in ultrasonic waves, and then fully oscillate and disperse in ultrasonic waves to form a uniform molecular sieve suspension after filtering. The pressure difference between the inner and outer sides of the basement membrane was adjusted to 0.0050 MPa, and the basement membrane was dip-coated in the prepared molecular sieve suspension for 120 seconds and then taken out. After drying, dry and solidify at a certain temperature ...

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Abstract

A method for synthesizing a type A molecular sieve membrane by evacuation and crystal coating method, the steps are: 1) introduce a layer of uniformly dispersed molecular sieve crystal seeds on the base membrane by using a vacuum pump to evacuate or compress with a compressor, and the evacuation or compression pressure is 0.0010 -0.0500Mpa, the dipping time is 30-300S, the concentration of the dipping solution is 1-20g / l, and the grain size is 0.20-10μm. 2) Synthesize A-type molecular sieve membrane by hydrothermal synthesis method and microwave synthesis method, and the solution composition of synthetic A-type molecular sieve membrane is: aNa2O:bAl2O3:5SiO2:cH2O, where a=(20-100), b=(0.5-5 ), c=(500-4000); hydrothermal or microwave synthesis, the temperature of hydrothermal synthesis is 323-373K, and the synthesis time is 2-60h; the temperature of microwave synthesis is 323-373K, and the synthesis time is 30-120min. The molecular sieve membrane synthesized by the method of the invention has good separation performance and high repeatability, and is suitable for industrial amplification.

Description

technical field [0001] The invention relates to a method for synthesizing a molecular sieve membrane, in particular to a method for synthesizing a type A molecular sieve membrane by means of an evacuation and crystal coating method. Background technique [0002] Molecular sieve is a microporous inorganic crystal material formed with silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron as the basic skeleton. Molecular sieves have the following advantages as inorganic membrane materials: 1) Molecular sieves have standardized and neat channels with a single pore size distribution; and the pore size of molecular sieves is similar to that of many important industrial raw materials. Molecules can be obtained by molecular sieving or type-selective diffusion. separate. 2) Molecular sieves have good chemical stability and thermal stability. 3) The diversity of molecular sieve structures leads to the diversity of its properties, such as different pore sizes and different hydro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D69/06B01D69/10B01D71/02C01B39/14
Inventor 杨维慎黄爱生刘杰李砚硕
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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