Method for preparing sapo-34 molecular sieve membrane by variable temperature method

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 of molecular sieve membrane thickness, etc., and achieve the effect of reducing mass transfer resistance and increasing permeability

Active Publication Date: 2017-09-29
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is simple to operate, but the quality of the membrane is affected by many factors, and repeated crystallization is required, which makes the molecular sieve membrane thicker
However, there is no literature report on the synthesis of SAPO-34 molecular sieve membranes by the variable temperature method.

Method used

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  • Method for preparing sapo-34 molecular sieve membrane by variable temperature method
  • Method for preparing sapo-34 molecular sieve membrane by variable temperature method
  • Method for preparing sapo-34 molecular sieve membrane by variable temperature method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The specific steps of preparing SAPO-34 molecular sieve membrane by the variable temperature method in this embodiment are as follows:

[0034] Step 1, add 2.46g of deionized water to 31.13g of tetraethylammonium hydroxide solution (TEAOH, 35wt%), then weigh 7.56g of aluminum isopropoxide and add it to the aforementioned solution, and stir at room temperature for 2-3 hours; then Add dropwise 1.665g silica sol (40wt%), stir 1 hour; Finally slowly add dropwise 8.53g phosphoric acid solution (H 3 PO 4 , 85wt%), stirred overnight. Microwave heating was used for crystallization at 180°C for 7h. After the product is taken out, it is centrifuged, washed and dried to obtain SAPO-34 molecular sieve seed crystals.

[0035] 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 ceram...

Embodiment 2

[0046] The difference from Example 1 is that in step 4, the time for continuing hydrothermal crystallization at 180° C. is 9 h. All the other steps are the same as in Example 1.

[0047] The surface and profile of gained SAPO-34 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 cubic crystals, and the cross-linking between the crystals is good (see figure a); the thickness of the film is relatively uniform, about 1.5 microns (see figure b).

[0048] The CO of the SAPO-34 molecular sieve membrane tube 2 / CH 4 The gas separation test results are shown in Table 2, at 4.0MPa, its CO 2 The permeability is 18.6×10 -7 mol / (m 2 s Pa), CO 2 / CH 4 The separation selectivity is 16.

[0049] The CO of the SAPO-34 molecular sieve membrane tube of table 2 embodiment 2 2 / CH 4 Gas Separation Test Results

[0050]

Embodiment 3

[0052] The difference from Example 1 is that in step 4, the time for continuing hydrothermal crystallization at 180° C. is 16.5 h. All the other steps are the same as in Example 1.

[0053] The surface and profile of gained SAPO-34 molecular sieve membrane are as follows Figure 4 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 good (see figure a); the thickness of the film is relatively uniform, about 3.5 microns (see figure b).

[0054] The CO of the SAPO-34 molecular sieve membrane tube 2 / CH 4 The gas separation test results are shown in Table 3, at 4.0MPa, its CO 2 The permeability is 19.5×10 -7 mol / (m 2 s Pa), CO 2 / CH 4 The separation selectivity is 24.

[0055] The CO of the SAPO-34 molecular sieve membrane of table 3 embodiment 3 2 / CH 4 Gas Separation Test Results

[0056]

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Abstract

The invention discloses a method for preparing a SAPO-34 molecular sieve membrane by a variable temperature method. The steps include: 1) synthesizing a SAPO-34 molecular sieve crystal seed; 2) uniformly coating the SAPO-34 molecular sieve seed crystal on a porous carrier; 3) preparing SAPO ‑34 molecular sieve membrane synthesis mother liquor; 4) immerse the porous carrier coated with SAPO‑34 molecular sieve seeds prepared in step 2) into the synthesis mother liquor for aging; 5) hydrothermal crystallization at 200-260°C for 0.1-5 hours , and then lower the temperature and continue the hydrothermal crystallization for 0.1 to 96 hours; 6) roast to remove the template agent to obtain a SAPO‑34 molecular sieve membrane. The invention utilizes a variable temperature method to prepare a thickness-controllable SAPO-34 molecular sieve membrane, successfully reduces the thickness of the molecular sieve membrane to 1 micron, thereby greatly reducing the mass transfer resistance of the SAPO-34 molecular sieve membrane and improving the permeability of the membrane.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of SAPO-34 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, the methods for preparing inorganic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08
Inventor 张延风李猛张建明曾高峰孙予罕孙长春李晋平孙志强冯永发
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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