Green synthesis method of ultra-thin SSZ-13 molecular sieve membrane

A green synthesis, molecular sieve technology, applied in molecular sieve and alkali exchange compounds, chemical instruments and methods, membrane technology, etc., can solve the problems of high unit price of membrane tube, unfavorable scale application, low permeability, etc., to improve permeability, reduce Equipment investment and the effect of reducing mass transfer resistance

Pending Publication Date: 2020-01-14
SHANGHAI UNIV OF ENG SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The synthesized molecular sieve membrane is relatively thick, usually about 5 microns, and the corresponding permea

Method used

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  • Green synthesis method of ultra-thin SSZ-13 molecular sieve membrane
  • Green synthesis method of ultra-thin SSZ-13 molecular sieve membrane
  • Green synthesis method of ultra-thin SSZ-13 molecular sieve membrane

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preparation example Construction

[0033] A green synthesis method of ultra-thin SSZ-13 molecular sieve membrane, by synthesizing SSZ-13 molecular sieve membrane at low temperature, using the characteristics that low temperature is conducive to nucleation and crystal growth rate is extremely slow, ultra-thin SSZ-13 is prepared Molecular sieve membrane (thickness to 500 nanometers), which greatly reduces mass transfer resistance and improves permeability. The synthesis temperature is lowered to ~100 degrees Celsius, and the SSZ-13 molecular sieve membrane can be synthesized under normal pressure, which avoids the use of high-pressure crystallization kettles and reduces equipment investment. The method includes:

[0034] 1) Mix the silicon source, ammonium trimethylammonium hydroxide and water, stir for 2 hours, then add hydrofluoric acid, the molar ratio of the reaction solution is: 1.0 SiO 2 :0.5HF:0.5TMAdaOH:3H 2 O (TMAdaOH: Trimethylammonium ammonium hydroxide), stirring for 30 minutes, to obtain a seed crys...

Embodiment 1

[0042] In this example, SSZ-13 molecular sieve membranes were synthesized by heating in a traditional oven. The specific steps are as follows:

[0043] Step 1: Synthetic formula of all-silicon CHA molecular sieve: 1.0SiO 2 :0.5HF:0.5TMAdaOH:3H 2 O (TMAdaOH: trimethylammonium adamantyl hydroxide). Mix ethyl orthosilicate and ammonium trimethyl ammonium hydroxide, stir for 4 hours, then remove excess water and ethanol in an oven at 80 degrees Celsius, then add hydrofluoric acid, and stir to obtain a synthetic mother liquor. Then crystallize at 453K for 24 hours to obtain an all-silicon CHA molecular sieve. The molecular sieve crystals are relatively large, about 8 microns. After being ball-milled by a ball mill, the crystals are pulverized to below 500 nanometers.

[0044] Step 2: Select a porous ceramic tube with a pore size of 100nm as the carrier, seal both ends of the carrier with glaze, wash and dry, seal the outer surface with PTFE tape, and brush the SAPO-34 molecular...

Embodiment 2

[0053] The difference from Example 1 is that in step 4, the crystallization kettle was placed in a 100°C oven for hydrothermal synthesis for 6 days, and the rest of the steps were the same as in Example 1.

[0054] 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 cubic crystals, and the cross-linking between the crystals is very good (see figure a); the thickness of the film is relatively uniform, about 610 nm (see figure b).

[0055] The CO of the SSZ-13 molecular sieve membrane tube 2 / CH 4 The gas separation test results are shown below, at 0.14MPa, its CO 2 The average value of the permeability is 45×10 -7 mol / (m 2 s Pa), CO 2 / CH 4 The average value of separation selectivity is 132. It can be seen that, compared with the traditional high-temperature synthesis in Example 1, the low-temperature synthesis can greatly...

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Abstract

The invention relates to a green synthesis method of an ultra-thin SSZ-13 molecular sieve membrane. The method comprises the steps: 1) preparing an all-silica CHA molecular sieve seed crystal, and performing ball milling so as to obtain a nano all-silica CHA seed crystal; 2) coating the nano all-silica CHA seed crystal on a porous carrier tube uniformly; 3) preparing an SSZ-13 molecular sieve membrane synthesis mother liquor; 4) putting the porous carrier tube obtained in the step 2) and the mother liquor obtained in the step 3) in a same crystallization kettle; 5) putting the crystallizationkettle in an oven for hydrothermal synthesis for 6-12 days at a synthesis temperature of 60-120 DEG C, washing the obtained membrane tube after completion of synthesis, and performing drying; and 6) performing high-temperature calcination for removal of a template so as to obtain the activated SSZ-13 molecular sieve membrane. The synthesis temperature is reduced greatly because the ultra-thin SSZ-13 molecular sieve membrane is synthesized at low temperature, use of a high-pressure crystallization kettle is avoided because the SSZ-13 molecular sieve membrane is synthesized under normal pressure, and meanwhile the thickness of the SSZ-13 molecular sieve membrane is reduced to 400-700 nm, so that the mass transfer resistance is reduced greatly, and the permeability is improved; and the methodcan also be applied to synthesis of other molecular sieve membranes.

Description

technical field [0001] The invention relates to a synthesis process of a molecular sieve membrane, in particular to a green synthesis method of an ultra-thin SSZ-13 molecular sieve membrane. Background technique [0002] Inorganic 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. [0003] At present, ...

Claims

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Application Information

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IPC IPC(8): C01B39/48B01D67/00B01D71/02
CPCC01B39/48B01D67/0039B01D71/028C01P2004/03
Inventor 张延风邱恒娥张野徐宁孔琳王明全
Owner SHANGHAI UNIV OF ENG SCI
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