Economic synthesis method of ultrathin SSZ-13 molecular sieve membrane

A synthesis method and molecular sieve technology, which is applied in the field of economical synthesis of ultra-thin SSZ-13 molecular sieve membranes, can solve problems such as the difficulty in preparing ultra-thin molecular sieve membranes, and achieve the effects of reducing synthesis costs, avoiding large-scale use, and high separation performance

Active Publication Date: 2020-04-24
SHANGHAI UNIV OF ENG SCI
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  • Abstract
  • Description
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Problems solved by technology

[0005] The purpose of the present invention is to provide an economical synthesis method of ultra-thin SSZ-13 molecular sieve membrane by recombination method in order to

Method used

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  • Economic synthesis method of ultrathin SSZ-13 molecular sieve membrane
  • Economic synthesis method of ultrathin SSZ-13 molecular sieve membrane
  • Economic synthesis method of ultrathin SSZ-13 molecular sieve membrane

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preparation example Construction

[0031] An economical synthesis method of ultra-thin SSZ-13 molecular sieve membrane, the seed crystal is loaded on the porous carrier, after template agent solution or molecular sieve membrane synthesis mother liquor is impregnated, only a small amount of liquid (template agent solution or molecular sieve membrane synthesis mother liquor, and There is no direct contact with the membrane tube), and the amorphous particles in the seed layer are converted into molecular sieve crystals at fixed points, and finally a continuous molecular sieve membrane is formed. The prepared SSZ-13 molecular sieve membrane thickness can be between 100 and 2000 nanometers, with extremely high CO 2 -CH 4 Separation performance, specifically comprising the following steps:

[0032] (1) Perform ball milling on the all-silicon CHA molecular sieve seed crystals. After ball milling, the molecular sieve crystals obtained from the CHA nanocrystal seeds are deeply fragmented and amorphous, and what are obt...

Embodiment 1

[0039] In this example, SSZ-13 molecular sieve membranes were synthesized by heating in a traditional oven. The specific steps are as follows:

[0040] Step 1: Synthetic formula of all-silicon CHA molecular sieve: 1.0SiO 2 :0.5HF:0.5TMAdaOH:3H 2 O (TMAdaOH: trimethylammonium adamantyl hydroxide). Ethyl orthosilicate and ammonium trimethylammonium hydroxide were mixed, stirred for 4 hours, then removed excess water and ethanol in an oven at 80 degrees Celsius, then added hydrofluoric acid, and stirred 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. Disperse the milled seed crystals in water to form a 0.1-0.4 wt% seed crystal dipping solution.

[0041] Step 2, select a porous ceramic tube with a pore size of 100nm as the carrier, seal the two e...

Embodiment 2

[0051] The difference from Example 1 is: in step 4, the porous carrier tube is immersed in 1.2 mol / liter ammonium trimethylammonium hydroxide solution (25wt%) for 1 minute, and in step 5, the crystallization kettle is put into 0.76g 25% TMAdaOH solution, all the other steps are the same as in Example 1.

[0052] The surface and profile of gained SSZ-13 molecular sieve membrane are as follows figure 2 shown, from figure 2 It can be seen that the surface of the carrier is completely covered by cubic crystals, and the cross-linking between the crystals is perfect (see figure a); the thickness of the film is relatively uniform, about 1.1 micron nm (see figure b).

[0053] The CO of the SSZ-13 molecular sieve membrane tube 2 / CH 4 The gas separation test results are shown in Table 1. Under 0.2MPa, the CO 2 The average value of the permeability is 21×10 -7 mol / (m 2 s Pa), CO 2 / CH 4 The average value of separation selectivity is 121.

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Abstract

The invention relates to an economic synthesis method of an ultrathin SSZ-13 molecular sieve membrane. The method comprises the following steps: loading a seed crystal on a porous carrier, dipping theporous carrier in a template solution or molecular sieve membrane synthesis mother liquor, carrying out crystallization in a crystallization kettle with only a small amount of liquid (the template solution or the molecular sieve membrane synthesis mother liquor is not in direct contact with the carrier), converting amorphous particles in a seed crystal layer into molecular sieve crystals at a fixed point, and finally forming a continuous molecular sieve membrane. Compared with the prior art, the method has the advantages that the ultrathin SSZ-13 molecular sieve membrane is synthesized, and the thickness of the membrane is effectively reduced to 200-500 nanometers, so that the mass transfer resistance is greatly reduced, and the permeability is improved. In addition, in a conventional hydrothermal method, a large amount of mother liquor is consumed, and the provided synthesis method reduces the using amount of mother liquor, greatly increases the utilization rate of raw materials, belongs to atom economic synthesis, and is also suitable for synthesis of other molecular sieve membranes.

Description

technical field [0001] The invention relates to the field of molecular sieve synthesis, in particular to an economical synthesis method of an ultrathin 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. Because the inorganic molecular sieve membrane has the advantages of uniform pore size, high temperature resistance, chemical solvent resistance and ion exchange, it has 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 prese...

Claims

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Application Information

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IPC IPC(8): C01B39/48C04B41/85B01D53/22B01D46/54B01D61/36B01D67/00
CPCC01B39/48C04B41/85C04B41/5024B01D53/228B01D46/543B01D61/362B01D67/0039B01D67/0051B01D67/0076C04B41/4552C04B41/4535Y02C20/40
Inventor 张延风王明全张野徐宁
Owner SHANGHAI UNIV OF ENG SCI
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