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Phosphorus-aluminum molecular sieve membrane synthesis method

A technology of aluminum phosphorus molecular sieve and synthesis method, which is applied in the field of molecular sieve membrane synthesis, and can solve problems such as limitations, difficulties, and narrow electrochemical window of solvent and water

Inactive Publication Date: 2015-06-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, if a continuous and dense molecular sieve membrane is to be prepared, the film must be further processed under hydrothermal conditions.
Since the high temperature and high pressure of the hydrothermal method must be carried out in a closed container, it is difficult to apply the electric field device to this system
At the same time, the electrochemical window of solvent water is very narrow (about 1.2V), and the applied voltage usually cannot exceed 2V to prevent water from being electrolyzed, so the application of this method in the synthesis of molecular sieve membranes is greatly limited.

Method used

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  • Phosphorus-aluminum molecular sieve membrane synthesis method
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  • Phosphorus-aluminum molecular sieve membrane synthesis method

Examples

Experimental program
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Effect test

Embodiment 1

[0040] The preparation of embodiment 1 phosphorus aluminum molecular sieve membrane

[0041] The synthesis solution for synthesizing molecular sieve membranes is prepared as follows:

[0042] Add 1.7 g of phosphoric acid and 0.2 g of HF into 32 g of 1-ethyl-3-methyl-imidazolium bromide ionic liquid, and heat and stir at 60° C. for 1 hour.

[0043] The substrate used in the synthesis of molecular sieve membranes is pure aluminum sheet with a purity of 99.99%, a length of 37mm, and a width of 18mm. Substrates were cleaned ultrasonically in acetone before use, and then dried with high-pressure air for later use.

[0044] Place two pure aluminum sheets vertically in an open reaction bottle as the working electrode and counter electrode respectively, and the reference electrode is Pt. Pour the synthesis solution into the reaction bottle, heat the system to 190°C, and use the constant potential method to set the voltage The temperature is -0.2V (vs. reference electrode), and the s...

Embodiment 2

[0045] The preparation of embodiment 2 phosphorus aluminum molecular sieve membrane

[0046] The same operation as in Example 1, except that the constant potential method was changed to a constant current test: the substrate used for the synthesis of molecular sieve membranes was a pure aluminum sheet with a purity of 99.99%, a length of 37 mm, and a width of 18 mm. Substrates were cleaned ultrasonically in acetone before use, and then dried with high-pressure air for later use.

[0047] Add 1.7 g of phosphoric acid and 0.2 g of HF into 32 g of 1-ethyl-3-methyl-imidazolium bromide ionic liquid, and heat and stir at 60° C. for 1 hour.

[0048] Place two pure aluminum sheets vertically in an open reaction bottle as the working electrode and counter electrode respectively, and the reference electrode is Pt. It is 10nA, and the synthesis time is 4h. The synthesized aluminum flakes were washed with deionized water, dried with high-pressure air, and then oven-dried at 60°C overnig...

Embodiment 3

[0049] The preparation of embodiment 3 aluminum phosphorus molecular sieve membrane

[0050] By the same operation as in Example 2, just change the test value of the constant current: the substrate used for the synthetic molecular sieve membrane is a pure aluminum sheet, the purity is 99.99%, the length is 37mm, and the width is 18mm. Substrates were cleaned ultrasonically in acetone before use, and then dried with high-pressure air for later use.

[0051] Add 1.7 g of phosphoric acid and 0.2 g of HF into 32 g of 1-ethyl-3-methyl-imidazolium bromide ionic liquid, and heat and stir at 60° C. for 1 hour.

[0052] Place two pure aluminum sheets vertically in an open reaction bottle as the working electrode and counter electrode respectively, and the reference electrode is Pt. It is 100nA, and the synthesis time is 4h. The XRD of the molecular sieve grown on the Al sheet of the working electrode confirmed that it has an AEL structure. The scanning electron micrographs showed tha...

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Abstract

The invention relates to a phosphorus-aluminum molecular sieve membrane synthesis method, wherein a three-electrode system or two-electrode system is adopted, a substrate and a synthesis liquid are placed in a reaction bottle, a constant potential method or linear scanning or pulsed current method or constant current method is adopted to carry out an electrochemical synthesis reaction, and the substrate is taken out and then is subjected to blow-drying after the reaction. According to the present invention, the synthesis method is simple and fast; the molecular sieve membrane synthesized by using the method has the good compactness; the molecular sieve membrane can be controllably synthesized by adjusting the synthesis parameters such as voltage, current, temperature, concentrations of each component in the synthesis liquid and the like; and the molecular sieve membrane synthesis method has high repeatability and is suitable for industrial scale-up.

Description

technical field [0001] The invention relates to the field of synthesis of molecular sieve membranes, and in particular provides a synthesis method of phosphorus aluminum molecular sieve membranes. Background technique [0002] Molecular sieves are a class of crystals with uniform pore size. Molecular sieve membranes assembled from molecular sieve crystals have broad application prospects in the fields of catalysis, separation, and ion exchange. Especially because of its low energy consumption, no pollution, high degree of separation and continuous separation, it has a very good application value in membrane separation. For example, in 1999, Japan introduced NaA molecular sieve membrane to the market for the dehydration of water-isopropanol and water-ethanol systems, realizing the industrial application of large-scale component devices of zeolite molecular sieve membrane for the first time. In the past ten years, due to its adjustable structure, controllable composition, go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D9/12C25D5/18
Inventor 蔡睿俞同文楚文玲刘延纯杨维慎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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