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Preparation method of SAPO-34 molecular sieve membrane

A technology of SAPO-34 and molecular sieve, applied in the field of preparation of SAPO-34 molecular sieve membrane, can solve the problems of inability to detect membrane tubes well, high price, restricting membrane engineering application, etc., to shorten synthesis time, improve quality, The effect of reducing the cost of synthesis

Active Publication Date: 2014-11-19
NANJING MEMBRANE IND TECH RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent US2011015057A1 discloses a method for preparing SAPO-34 molecular sieve membranes on the inner wall of an asymmetric alumina tube. Although the synthesis temperature is reduced to 200°C, the synthesis time still takes 20 hours
The above-mentioned SAPO-34 molecular sieve membranes all use asymmetric alumina supports, which are expensive and restrict the engineering application of the membranes.
Moreover, these SAPO-34 molecular sieve membranes are all grown on the inner wall of the porous support, and there are detection problems in the use of large-scale membrane modules: that is, when a membrane tube has a problem, it cannot be detected well because the permeated components are mixed together. problem membrane tube

Method used

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  • Preparation method of SAPO-34 molecular sieve membrane
  • Preparation method of SAPO-34 molecular sieve membrane
  • Preparation method of SAPO-34 molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of SAPO-34 seed crystals: mix the template agent tetraethylammonium hydroxide for short TEAOH, aluminum n-butoxide, phosphoric acid, silicon source chabazite and water, and after aging for 1 hour at room temperature, the formed sol The molar ratio of the components is: P 2 o 5 / Al 2 o 3 = 0.7, SiO 2 / Al 2 o 3 =0.5, TEAOH / Al 2 o 3 =1.8,H 2 O / Al 2 o 3 =70. The sol was added into a polytetrafluoroethylene-lined stainless steel reactor, hydrothermally synthesized at a synthesis temperature of 190° C. for 2 hours, and cleaned by centrifugation to obtain a SAPO-34 molecular sieve.

[0031] (2) Support body pretreatment: Porous mullite tube is used as the support body for membrane synthesis, and the molar ratio is 66% Al 2 o 3 and 34% SiO 2 . The inner and outer diameters are 9mm and 12mm respectively, the length is 100mm, the average pore diameter is about 1.0μm, and the porosity is about 30%. The outer wall of the support body was pretreated w...

Embodiment 2

[0039] (1) Preparation of seed crystals: the preparation process is the same as step (1) in Example 1, except that aluminum foil is selected as the aluminum source, and the molar ratio of the sol is P 2 o 5 / Al 2 o 3 = 0.9, SiO 2 / Al 2 o 3 =0.05, TEAOH / Al 2 o 3 = 1.5, H 2 O / Al 2 o 3 =40.

[0040] (2) Support body pretreatment: the preparation process is the same as step (2) of Example 1, except that the seed crystal content in the seed crystal suspension is 2% of the solution mass, and the pH value is adjusted to 10 by using sodium hydroxide aqueous solution.

[0041] (3) Synthesis of SAPO-34 molecular sieve membrane: the preparation process is the same as step (3) of Example 1, except that aluminum powder is selected as the aluminum source.

[0042] The prepared membrane M2 was used at 25°C, CO 2 / CH 4 The gas separation performance was characterized in the (50 / 50) system, and the results of the gas separation experiment are shown in Table 1.

Embodiment 3

[0044] (1) Preparation of seed crystals: the preparation process is the same as step (1) of Example 1, except that aluminum hydroxide is selected as the aluminum source, and the sol is aged at room temperature for 12 hours.

[0045] (2) support body pretreatment: the preparation process is the same as step (2) of embodiment 1, the difference is that the 5% polydiallyldimethylamine sulfate solution whose mass concentration is the total mass of the solution is used, and the immersion time is 0.5 Hour.

[0046] (3) Synthesis of SAPO-34 molecular sieve membrane: the preparation process is the same as step (3) in Example 1, except that aluminum isopropoxide is selected as the aluminum source.

[0047] The prepared membrane M3 was used at 25°C, CO 2 / CH 4 The gas separation performance was characterized in the (50 / 50) system, and the results of the gas separation experiment are shown in Table 1.

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Abstract

The invention provides a preparation method of a SAPO-34 molecular sieve membrane. The method is characterized in that a specific zeolite molecular sieve is employed as a silicon source. A continuous compact SAPO-34 molecular sieve thin film is formed on a surface of a porous ceramic supporting body, namely, a layer of the SAPO-34 molecular sieve membrane is grown on the porous ceramic supporting body with a crystalline state zeolite molecular sieve being the silicon source. A structure unit of the molecular sieve is same as that of SAPO-34. Crystal nucleus are provided for crystallization of a SAPO-34 molecular sieve and a synthesis time of the membrane is shortened. In addition, the content of silicon in the SAPO-34 molecular sieve membrane can be adjusted within a large range. The membrane has a preferable selectivity on CO2 and a high permeation flux and separation selectivity when being used for separating mixing systems of CO2 / CH4.

Description

technical field [0001] The invention provides a preparation method of a SAPO-34 molecular sieve membrane, which belongs to the field of preparation and application of molecular sieve membrane materials. Background technique [0002] Carbon dioxide is the main impurity gas of natural gas (the effective component is methane), which not only reduces the combustion calorific value of natural gas, but also causes corrosion to gas pipelines under wet conditions. Common organic amines (such as methyldiethanolamine) absorption separation process has the disadvantages of high energy consumption and large amount of reagents. Using membrane technology to separate carbon dioxide from natural gas can reduce the cost of natural gas purification. with CO 2 Selective polymer membranes such as cellulose acetate and polyimide membranes are used for industrial natural gas separation. As early as the 1980s, developed countries such as the United States and Europe have used cellulose acetate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 周荣飞徐南平仲盛来戴继东
Owner NANJING MEMBRANE IND TECH RES INST CO LTD
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