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Constant current synthesis method for phosphorus aluminum molecular sieve membrane

A kind of technology of phosphorus aluminum molecular sieve and synthesis method, applied in the direction of electrodes, electrolysis process, electrolysis components, etc., can solve the problems of narrow, limited and difficult 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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  • Constant current synthesis method for phosphorus aluminum molecular sieve membrane
  • Constant current synthesis method for phosphorus aluminum molecular sieve membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation of embodiment 1 phosphorus aluminum molecular sieve membrane

[0025] 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.

[0026] 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.

[0027] 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 overnight. The XRD of the molecular sieve grown on the Al sheet of the working electrode confirmed the AEL structure, and the scan...

Embodiment 2

[0028] The preparation of embodiment 2 phosphorus aluminum molecular sieve membrane

[0029] By the same operation as in Example 1, just change the test value of the constant current: 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.

[0030] 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.

[0031] 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...

Embodiment 3

[0032] Embodiment 3 anticorrosion performance test

[0033] The etching solution is 0.1M NaCl aqueous solution. Pour the corrosion solution into the corrosion pool, the working electrode is a bare aluminum sheet or the molecular sieve membrane prepared in Example 2, the counter electrode is a Pt sheet, and the reference electrode is (Ag.AgCl) / KCl (3.5M). Before the corrosion test, the molecular sieve was stabilized in the corrosion solution for 30 minutes, and then the DC polarization curve was scanned, the scanning range was -0.5V to 0.5V, and the scanning speed was 10mV / min. The result is as figure 2 shown. It is shown that the dense, highly in-plane and in-plane oriented molecular sieve membranes synthesized by electrochemical methods have excellent anti-corrosion properties.

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Abstract

The invention relates to a constant current synthesis method for a phosphorus aluminum molecular sieve membrane. The method includes: adopting a three-electrode system or two-electrode system, placing a substrate and a synthetic liquid in a reaction bottle, carrying out electrochemical synthesis reaction by a constant current technique, taking out the substrate after the reaction, and performing blow-drying and stoving. The synthesis method provided by the invention is simple and rapid. The molecular sieve membrane synthesized by the method provided by the invention has good compactness, and by adjusting the synthesis parameters, like current, temperature, concentration of each synthetic liquid component and the like, controllable synthesis of the molecular sieve membrane can be achieved. The molecular sieve membrane synthesis method is highly reproducible and is 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 current 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, controllabl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/00C25B11/04
CPCC25B1/00C25B11/051
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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