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Phosphorus aluminum molecular sieve membrane potentiostatic synthesis method

A phospho-aluminum molecular sieve and a synthesis method are applied in the field of synthesis of molecular sieve membranes, and can solve the problems of narrow, difficult, and limited electrochemical window of solvent 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 potentiostatic synthesis method
  • Phosphorus aluminum molecular sieve membrane potentiostatic synthesis method
  • Phosphorus aluminum molecular sieve membrane potentiostatic synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Preparation of Aluminum Phosphorus Molecular Sieve Membrane

[0033] The synthesis solution for synthesizing molecular sieve membranes is prepared as follows:

[0034] 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.

[0035] 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.

[0036] 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 synthesi...

Embodiment 2

[0037] Example 2 Preparation of Aluminum Phosphorus Molecular Sieve Membrane

[0038] According to the same operation as in Example 1, just change the electrochemical synthesis time: the substrate used for synthesizing the molecular sieve membrane is 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.

[0039] 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.

[0040] 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 It is -0.2V (vs. reference electrode), and the synthesis time is 6h...

Embodiment 3

[0041] Example 3 Preparation of Aluminum Phosphorus Molecular Sieve Membrane

[0042] According to the same operation as in Example 1, just change the composition of the synthetic liquid: the substrate used for the synthetic molecular sieve membrane is 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.

[0043] Add 0.51 g of phosphoric acid and 0.06 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.

[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 It is -0.2V (vs. reference electrode), and the synthesis time i...

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Abstract

A phosphorus aluminum molecular sieve membrane potentiostatic synthesis method, a three electrode system or a two electrode system is used, a substrate and a synthetic liquid are placed in a reaction flask for electrochemical synthesis reaction by potentiostatic method, and after the reaction, the substrate is taken out, blow-dried and baked. The synthesis method is simple and fast. The molecular sieve membrane prepared by the method has good compactness, and can be controllably prepared by adjusting of the synthesis parameters comprising voltage, temperature, concentration of each component of the synthesis liquid. The molecular sieve membrane synthesis method is highly reproducible and suitable for industrial amplification.

Description

technical field [0001] The invention relates to the field of synthesis of molecular sieve membranes, and in particular provides a constant potential 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, controlla...

Claims

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Application Information

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IPC IPC(8): C25D9/12
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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