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Method for preparing ion exchange SAPO-34 molecular sieve membrane

A SAPO-34, ion exchange technology, applied in the direction of molecular sieve and alkali exchange phosphate, chemical instruments and methods, membrane technology, etc., can solve the problems of decreased permeability, reduce synthesis cost, simplify the preparation process, and improve separation performance and reproducible effects

Inactive Publication Date: 2014-01-15
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Hong et al. used Li + 、Na + 、K + , NH 4 + and Cu 2+ Ion-exchange the calcined H-SAPO-34 molecular sieve membrane in a non-aqueous solution to make CO 2 / CH 4 Separation selectivity increased by 60%, but CO 2 Permeability decreased [Microporous Mesoporous Mater.106(2007)140–146]

Method used

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  • Method for preparing ion exchange SAPO-34 molecular sieve membrane
  • Method for preparing ion exchange SAPO-34 molecular sieve membrane
  • Method for preparing ion exchange SAPO-34 molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1 does not pass through ion exchange, roasts under vacuum condition and prepares SAPO-34 molecular sieve membrane

[0026] Step 1: Add 2.46g of deionized water to 31.13g of tetraethylammonium hydroxide solution (TEAOH, 35%), then weigh 7.56g of aluminum isopropoxide into the aforementioned solution, and stir at room temperature for 2-3 hours; then Add 1.665g of silica sol (40%) dropwise and stir for 1 hour; finally slowly add 8.53g of phosphoric acid solution (H 3 PO 4 , 85%), stirred overnight. Microwave heating was used for crystallization at 180°C for 7 hours. After the product is taken out, it is centrifuged, washed, and dried to obtain SAPO-34 molecular sieve seed crystals.

[0027] 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 sieve seed crystal to the inner surface of the ceramic tube.

[00...

Embodiment 2

[0037] Embodiment 2 Soak with 1% sodium nitrate solution, prepare Na-SAPO-34 molecular sieve membrane by vacuum roasting

[0038] The difference from Example 1 is that after step 3 is completed and before step 4 is performed, the molecular sieve membrane tube prepared in step 3 is soaked in 1% sodium nitrate solution for 10 minutes, and then put into an oven for drying. All the other steps are the same as in Example 1.

[0039] CO 2 / CH 4 The gas separation test method is the same as in Example 1, and the test results are shown in Table 3. CO 2 / CH 4 The separation selectivity of the mixed gas is 81, which is 40% higher than that of the SAPO-34 molecular sieve membrane without ion exchange in Example 1.

[0040] Table 3 CO of Example 2 2 / CH 4 Gas Separation Test Results

[0041]

[0042] Note: The pressure difference between the feed side and the permeate side of the membrane tube is 3.99MPa

Embodiment 3

[0043] Example 3 Soak with 1% potassium nitrate solution, prepare K-SAPO-34 molecular sieve membrane by vacuum roasting

[0044] The difference from Example 1 is that after step 3 is completed and before step 4 is carried out, the molecular sieve membrane tube prepared in step 3 is soaked in 1% potassium nitrate solution for 3 minutes, and then put into an oven for drying. All the other steps are the same as in Example 1.

[0045] CO 2 / CH 4 The gas separation test method is the same as in Example 1, and the test results are shown in Table 4. CO 2 / CH 4 The separation selectivity of the mixed gas is 73, which is 26% higher than that of the SAPO-34 molecular sieve membrane without ion exchange in Example 1.

[0046] Table 4 CO of Example 3 2 / CH 4 Gas Separation Test Results

[0047]

[0048] Note: The pressure difference between the feed side and the permeate side of the membrane tube is 3.99MPa

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Abstract

The invention discloses a method for preparing ion exchange SAPO-34 molecular sieve membrane, comprising the following steps of: (1) synthesizing SAPO-34 molecular sieve seeds; (2) loading the SAPO-34 molecular sieve seeds on a porous carrier; (3) synthesizing a SAPO-34 molecular sieve membrane; (4) loading a metal salt with a melting point lower than a roasting temperature in a step (5) on the SAPO-34 molecular sieve membrane; and (5) high temperature roasting to remove a template, and simultaneously carrying out ion exchange to obtain the ion exchange SAPO-34 molecular sieve membrane. By loading metal salts with a low melting point on the surface of the molecular sieve membrane, the method combines two steps: template removal and ion exchange, into one step, thereby simplifying a preparation process of the SAPO-34 molecular sieve membrane, reduces synthesis cost, and simultaneously raising gas separating performance of the SAPO-34 molecular sieve membrane.

Description

technical field [0001] The invention relates to the technical field of chemical separation, in particular to a method for preparing an ion-exchange SAPO-34 molecular sieve membrane. Background technique [0002] Natural gas is an important energy and chemical raw material alongside petroleum and coal. The global annual consumption of natural gas is nearly 3 trillion cubic meters per year, accounting for 23.7% of the total energy demand. [0003] Natural gas usually contains some impurities, such as water, carbon dioxide, nitrogen, hydrogen sulfide, etc. All natural gas is treated to varying degrees in order to meet pipeline requirements. Natural gas purification is currently the largest industrial gas treatment process, the global market is about 5 billion US dollars per year, mainly to remove CO from natural gas 2 . According to statistics, more than 20% of the natural gas in the United States is due to excessive CO 2 content and require advanced processing. CO in She...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D67/00C01B39/54
Inventor 孙予罕张延风李猛
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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