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Preparation method of high-performance SAPO (silicoaluminophosphate)-34 molecular sieve membrane

A technology of SAPO-34 and molecular sieve, which is applied in the field of preparation of SAPO-34 molecular sieve membrane, can solve the problems that the preparation repeatability needs to be further improved, and achieve the effect of improving synthesis repeatability, uniformity and stability

Inactive Publication Date: 2014-07-02
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the preparation method for preparing SAPO-34 molecular sieve membrane and the performance and preparation repeatability of the prepared SAPO-34 molecular sieve membrane still need to be further improved.

Method used

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  • Preparation method of high-performance SAPO (silicoaluminophosphate)-34 molecular sieve membrane
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  • Preparation method of high-performance SAPO (silicoaluminophosphate)-34 molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The SAPO-34 molecular sieve membrane preparation when the mol ratio of embodiment 1 hydrofluoric acid and aluminum oxide is 0.05

[0042] Step 1: Add 2.46g of deionized water to 31.13g of tetraethylammonium hydroxide solution (TEAOH, 35wt%), 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 (40wt%) dropwise and stir for 1 hour; finally slowly add 8.53g of phosphoric acid solution (H 3 PO 4 , 85wt%), stirred overnight. Microwave heating was used for crystallization at 180°C for 7 hours. After the product was taken out, it was centrifuged, washed with deionized water, and dried to obtain SAPO-34 molecular sieve seed crystals. The SEM image of the seed crystal, such as figure 1 As shown, the seed crystal is a 300×300×100 nmde plate crystal. The XRD pattern of the seed crystal, such as figure 2 As shown, it is a pure SAPO-34 crystal phase without miscellaneous crystals...

Embodiment 2

[0053] The preparation of SAPO-34 molecular sieve membrane when the mol ratio of embodiment 2 hydrofluoric acid and aluminum oxide is 0.1

[0054] The difference from Example 1 is that in Step 3, 0.09g of hydrofluoric acid (HF, 40wt%) was added; 8.56g of tetraethylammonium hydroxide solution (TEAOH, 35wt%) was added. All the other steps are the same as in Example 1.

[0055] CO 2 / CH 4 The gas separation test method is the same as in Example 1, and the test results are shown in Table 2. image 3 with Figure 4 It is the surface and section SEM images of the prepared SAPO-34 molecular sieve membrane. image 3 In , it is shown that the surface of the carrier is completely covered by SAPO-34 crystals, and the cross-linking between crystals is perfect. Figure 4 In , it is shown that the thickness of the SAPO-34 molecular sieve membrane is about 8 microns.

[0056] Table 2 CO of Example 2 2 / CH 4 Gas Separation Test Results

[0057]

[0058] Note: The pressure differen...

Embodiment 3

[0059] The preparation of SAPO-34 molecular sieve membrane when the molar ratio of hydrofluoric acid and aluminum oxide in embodiment 3 is 0.15

[0060] The difference from Example 1 is that 0.135g of hydrofluoric acid (HF, 40wt%) is added in step 3. All the other steps are the same as in Example 1.

[0061] 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.

[0062] Table 3 CO of Example 3 2 / CH 4 Gas Separation Test Results

[0063]

[0064] 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 preparation method of a high-performance SAPO (silicoaluminophosphate)-34 molecular sieve membrane. The preparation method comprises the following steps: (1) obtaining an SAPO-34 molecular sieve crystal seed; (2) coating the SAPO-34 molecular sieve crystal seed on the inner surface of a porous carrier; (3) putting the prepared porous carrier coated with the SAPO-34 molecular sieve crystal seed into synthesizing mother liquor of the molecular sieve membrane and synthesizing an SAPO-34 molecular sieve membrane tube; (4) roasting to remove a template agent, thereby obtaining the SAPO-34 molecular sieve membrane without the template agent. The preparation method disclosed by the invention has the advantages that the uniformity and stability of the synthesizing mother liquid are greatly improved, the synthesis repeatability of the SAPO-34 molecular sieve membrane is improved, and the synthesized SAPO-34 molecular sieve membrane has higher gas permeability and CO2 / CH4 selectivity. Furthermore, the SAPO-34 molecular sieve membrane prepared by the preparation method can be applied to gas separation of CO2-CH4, CO2-H2 and CO2 / N2 and the like.

Description

technical field [0001] The invention relates to a preparation method of a SAPO-34 molecular sieve membrane, in particular to a preparation method of a high-performance SAPO-34 molecular sieve membrane. Background technique [0002] Natural gas is an important energy and chemical raw material alongside petroleum and coal. The content of methane, the main component in natural gas, is usually 75% to 90%. In addition, it also contains hydrocarbons such as ethane, propane, butane, and other impurities, including water, carbon dioxide, nitrogen, hydrogen sulfide, etc. The existence of these impurities seriously affects the storage and transportation of natural gas and needs to be strictly controlled. As a result, the world spends $5 billion per year on natural gas purification, mainly to remove CO from natural gas 2 . According to statistics, more than 20% of the natural gas fields in the United States are due to excessive CO 2 content and require advanced processing. CO in S...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54B01D53/22C10L3/10
CPCY02C20/20Y02C10/10Y02C20/40Y02P20/151
Inventor 张延风李猛孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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