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Method of exhausting and in-situ hydrothermally synthesizing type-A molecular sieve film

An in-situ hydrothermal and molecular sieve technology, which is applied in chemical instruments and methods, A-type crystalline aluminosilicate zeolite, membrane technology, etc. Different levels of difficulty, etc., to achieve the effect of increasing the speed, reducing the synthesis time, and improving the synthesis speed

Inactive Publication Date: 2006-09-13
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

In this way, on the one hand, in a relatively short period of time, the surface of the basement membrane cannot form a dense and continuous molecular sieve film due to the lack of sufficient molecular sieve grains, but prolonging the time of hydrothermal synthesis will inevitably lead to the occurrence of crystal transformation; on the other hand Most of the molecular sieve grains are deposited to the bottom of the reactor due to gravity, causing great waste (research shows that the utilization rate of molecular sieve grains is only 20-30%), especially as the synthesis time increases, the crystal nucleus or molecular sieve The longer the grain grows, the greater the negative effect of gravity
In addition, gravity makes the crystal nuclei or molecular sieve crystals migrate and adsorb to the surface of the basement membrane in different directions, and the thickness of the molecular sieve membrane formed at the upper and lower ends is very different. Therefore, it is difficult to form a uniform and continuous molecular sieve membrane on the surface of the basement membrane.

Method used

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  • Method of exhausting and in-situ hydrothermally synthesizing type-A molecular sieve film
  • Method of exhausting and in-situ hydrothermally synthesizing type-A molecular sieve film
  • Method of exhausting and in-situ hydrothermally synthesizing type-A molecular sieve film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Step 1 Basement Membrane Preparation

[0038] α-Al used in the experiment 2 o 3The base membrane is prepared by casting method, the outer diameter of the membrane tube is 10mm, the inner diameter is 7mm, the length is 260mm, the pore radius is 0.5-1.0μm, and the porosity is about 50%. The base film was smoothed with fine sandpaper, ultrasonically washed in distilled water, and treated at high temperature for later use.

[0039] Step 2 Reaction solution preparation

[0040] Weigh a certain amount of NaOH and dissolve it in distilled water, add aluminum foil after clarification, and stir to form an aluminum solution; measure a certain amount of silica sol and add it to pre-heated distilled water, stir well; slowly add the pre-heated aluminum solution to the silica sol , continue stirring for a few minutes. The composition (molar ratio) of each component in the final solution is 50Na 2 O:Al 2 o 3 : 5SiO 2 : 1000H 2 O.

[0041] Step 3: Evacuate in-situ hydrotherma...

Embodiment 2

[0044] Step 1 Basement Membrane Preparation

[0045] Same as example 1.

[0046] Step 2 Reaction solution preparation

[0047] Repeat Step 2 of Example 1.

[0048] Step 3: Evacuate in-situ hydrothermal synthesis of type A molecular sieve membrane

[0049] After the basement membrane is fixed, place it vertically in the evacuated in-situ hydrothermal synthesis reactor, adjust the pressure difference between the inside and outside of the basement membrane tube to 0.0150MPa, and evacuate for 200Min; pour the reaction solution, and perform the in-situ hydrothermal synthesis at 363K for 2 to 8 hours Take it out, cool it to room temperature, wash it with distilled water until neutral, dry it and use it for characterization and pervaporation experiments.

Embodiment 3

[0051] Step 1 Basement Membrane Preparation

[0052] Same as example 1.

[0053] Step 2 Reaction solution preparation

[0054] Repeat Step 2 of Example 1

[0055] Step 3: Evacuate in-situ hydrothermal synthesis of type A molecular sieve membrane

[0056] After the basement membrane is fixed, place it vertically in the evacuated in-situ hydrothermal synthesis reactor, adjust the pressure difference between the inside and outside of the basement membrane tube to 0.0200MPa, and compress for 500Min; pour the reaction solution, and then evacuate the in-situ hydrothermal synthesis at 363K for 2 to 8 hours Take it out, cool it to room temperature, wash it with distilled water until neutral, dry it and use it for characterization and pervaporation experiments.

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Abstract

The method of exhausting and in-situ hydrothermally synthesizing type-A molecular sieve film includes: pumping with water pump or compressing with compressor to make the crystal kernel formed in the synthetic liquid migrate fast to the surface of the base film to speed the synthesis of type-A molecular sieve film, with the pumping or compressing pressure being 0.0005-0.0500 MPa and the pumping or compressing time being 10-500 min; and hydrothermally synthesizing type-A molecular sieve film in the solution comprising Na2O in 20-100 portions, Al2O3 in 0.5-5 portions, SiO2 in 5 portions and H2O in 500-4000 portions at 323-373 K for 1-60 hr. The present invention has obviously reduced molecular sieve film synthesizing time and raised material utilization, and the synthesized molecular sieve film is homogeneous, compact and continuous.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieve membranes, and in particular provides a method for quickly synthesizing high-performance molecular sieve membranes by means of water pump evacuation or compressor compression. 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: [0003] 1) Molecular sieves have well-regulated pores with a single pore size distribution; and the pore size of molecular sieves is similar to the molecular size of many important industrial raw materials, and molecules can be separated by molecular sieving or type-selective diffusion. [0004] 2) Molecular sieves have good chemical stability and thermal stability. [0005] 3) The diversity of molecular sieve structures leads to the diversity of its p...

Claims

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Application Information

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