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Method for synthesizing DDR molecular sieve membrane

A molecular sieve and synthetic mother liquor technology, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve problems such as hindering the industrial application of DDR molecular sieve membranes, and achieve the effects of shortening synthesis time, increasing crystallization rate, and increasing alkalinity.

Inactive Publication Date: 2019-12-24
SHANGHAI UNIV OF ENG SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, increasing the synthesis temperature leads to the formation of heterogeneous phases
These unfavorable conditions have greatly hindered the industrial application of DDR molecular sieve membranes.

Method used

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  • Method for synthesizing DDR molecular sieve membrane
  • Method for synthesizing DDR molecular sieve membrane
  • Method for synthesizing DDR molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A method for synthesizing DDR molecular sieve membranes with a molar ratio of 1SiO 2 :50H 2 O:0.4Adam:0.2TEAOH mother liquor, crystallized at 220°C for 2 hours to prepare all-silicon DDR molecular sieve membrane.

[0035] In this example, SSZ-13 molecular sieve membranes were synthesized by heating in a traditional oven. The specific steps are as follows:

[0036] Step 1: Synthetic formula of all-silicon DDR molecular sieve: 1.0SiO 2 :4.0EDA:0.5ADA:100H 2 O (EDA: ethylenediamine, ADA: amantadine). Mix ethylenediamine, water and adamantane ammonium, stir for 1 hour, then add ethyl orthosilicate, stir overnight at room temperature to obtain a synthetic mother liquor. Crystallize at 433K for 24 days to obtain an all-silicon DDR molecular sieve. The molecular sieve crystals are relatively large, about 8 microns. After being milled by a ball mill, the crystals are crushed to below 500 nanometers.

[0037]Step 2: Select a porous ceramic tube with a pore size of 100nm a...

Embodiment 2

[0046] A method for synthesizing a DDR molecular sieve membrane, the difference from Example 1 is: crystallization at 220° C. for 4 hours to prepare an all-silicon DDR molecular sieve membrane. All the other steps are the same as in Example 1.

[0047] The surface and profile of gained SSZ-13 molecular sieve membrane are as follows figure 2 As shown in the figure, it can be seen from the figure that the surface of the carrier is completely covered by diamond-shaped DDR crystals, and the cross-linking between the crystals is very good (see figure a); the thickness of the film is relatively uniform, about 8.9 microns (see figure b).

[0048] The CO of the SSZ-13 molecular sieve membrane tube 2 / CH 4 The gas separation test results are shown below, at 0.2MPa, its CO 2 The average value of the permeability is 0.78×10 -7 mol / (m 2 s Pa), CO 2 / CH 4 The average separation selectivity is 165.

Embodiment 3

[0050] A method for synthesizing a DDR molecular sieve membrane, the difference from Example 1 is: crystallization at 220° C. for 3 hours to prepare an all-silicon DDR molecular sieve membrane. All the other steps are the same as in Example 1.

[0051] The surface and profile of gained DDR molecular sieve membrane are as follows image 3 As shown in the figure, it can be seen from the figure that the surface of the carrier is completely covered by diamond-shaped DDR crystals, and the cross-linking between the crystals is very good (see figure a); the thickness of the film is relatively uniform, about 4.3 microns (see figure b).

[0052] The DDR molecular sieve membrane tubes CO 2 / CH 4 The gas separation test results are shown below, at 0.2MPa, its CO 2 The average value of the permeability is 1.5×10 -7 mol / (m 2 s Pa), CO 2 / CH 4 The average separation selectivity is 155.

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Abstract

The invention relates to a method for synthesizing a DDR molecular sieve membrane. The method comprises the following steps: carrying out ball milling on DDR molecular sieve powder to obtain submicronDDR molecular sieve seed crystals; mixing a silicon source, amantadine, tetraethylammonium hydroxide and water to obtain DDR molecular sieve membrane synthesis mother liquor; coating a porous carriertube with the DDR molecular sieve seed crystals; putting the DDR molecular sieve membrane synthesis mother liquor and the porous carrier tube into a crystallization kettle for hydrothermal synthesistreatment, and washing and drying an obtained membrane tube after synthesis is finished; and roasting the membrane tube in an ozone atmosphere to remove the tetraethylammonium hydroxide to obtain an activated DDR molecular sieve membrane. Compared with the prior art, the method utilizes a mixed template agent consisting of the amantadine and the tetraethylammonium hydroxide, and the addition of the tetraethylammonium hydroxide inhibits generation of impurities, so that the DDR molecular sieve membrane can be rapidly synthesized at high temperature, the crystallization time is greatly shortened, and the obtained DDR molecular sieve membrane has relatively high CO2-CH4 separation selectivity.

Description

technical field [0001] The invention relates to a preparation method of a molecular sieve membrane, in particular to a method for synthesizing a DDR molecular sieve membrane. Background technique [0002] Molecular sieve membrane is obtained by preparing a layer of continuous, dense and uniform molecular sieve on a porous carrier. Due to the advantages of uniform pore size, high temperature resistance, chemical solvent resistance and ion exchange, inorganic molecular sieve membranes have great application potential in the fields of membrane catalytic reaction, gas separation, liquid pervaporation separation and environmental protection. For example, in CO 2 In the field of removal, because the membrane separation device has the advantages of low energy consumption, continuous operation, low equipment investment, small volume, and easy maintenance, it is very suitable for high CO 2 The harsh separation environment of content. DDR molecular sieve (the structure code of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D69/04B01D71/02C01B32/50C10L3/10B01D53/22
CPCB01D53/228B01D67/0039B01D69/04B01D71/028B01D2256/245B01D2257/504C10L3/104C10L2290/548C01B32/50Y02C20/20Y02P20/151Y02C20/40
Inventor 张延风徐宁王明全张野孔琳
Owner SHANGHAI UNIV OF ENG SCI
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