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Method for ionothermal synthesis of aluminum phosphate AlPO4-n zeolite membranes

A technology of ionothermal synthesis and alpo4-n, which is applied in the synthesis and application of molecular sieve membranes, can solve the problems of rare molecular sieve membranes and achieve excellent anti-corrosion performance and high repeatability

Active Publication Date: 2013-06-19
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

There is still very little research on the preparation of molecular sieve membranes in ionic liquids

Method used

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  • Method for ionothermal synthesis of aluminum phosphate AlPO4-n zeolite membranes
  • Method for ionothermal synthesis of aluminum phosphate AlPO4-n zeolite membranes
  • Method for ionothermal synthesis of aluminum phosphate AlPO4-n zeolite membranes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 AlPO 4 Preparation of -11 molecular sieve membrane

[0029]The substrate used for synthesizing the molecular sieve membrane is a pure aluminum sheet with a purity of 99.99%, a length of 37mm, and a width of 18mm. The substrate is ultrasonically washed in acetone before use, and then dried with high-pressure air for use.

[0030] The synthesis solution for synthesizing molecular sieve membranes is configured as follows:

[0031] 1.72 g of phosphoric acid (85%) and 0.2 g of HF (40%) were added to 30.57 g of 1-ethyl-3-methyl-imidazolium bromide ionic liquid, heated and stirred at 90° C. for 1 hour.

[0032] Place the pure aluminum sheet vertically in the polytetrafluoroethylene synthesis kettle, pour the synthesis liquid into the synthesis kettle, wrap the heating jacket on the outside of the synthesis kettle, heat it up to 190°C, and keep heating at this temperature for 4 hours; The synthesized aluminum flakes were washed with deionized water, dried with high...

Embodiment 2

[0033] Example 2 AlPO 4 Preparation of -11 molecular sieve membrane

[0034] By the same operation of Example 1, just change the heating temperature of the synthetic liquid: 1.72 gram of phosphoric acid (85%) and 0.2 gram of HF (40%) are added to 30.57 gram of 1-ethyl-3-methyl-imidazolium bromide ionic liquid , heated and stirred at 90°C for 1 hour. Place the pure aluminum sheet vertically in the polytetrafluoroethylene synthesis kettle, pour the synthesis liquid into the synthesis kettle, wrap the heating jacket on the outside of the synthesis kettle, heat it up to 150°C, and keep heating at this temperature for 4 hours; The synthesized aluminum flakes were washed with deionized water, dried with high-pressure air, and then oven-dried at 60°C overnight. The obtained molecular sieve was confirmed to have an AEL structure by X-ray diffraction, but the compactness of the film was poor.

Embodiment 3

[0035] Example 3 AlPO 4 Preparation of -11 molecular sieve membrane

[0036] By the same operation of Example 1, just change the heating temperature of the synthetic liquid: 1.72 gram of phosphoric acid (85%) and 0.2 gram of HF (40%) are added to 30.57 gram of 1-ethyl-3-methyl-imidazolium bromide ionic liquid , heated and stirred at 90°C for 1 hour. Place the pure aluminum sheet vertically in the polytetrafluoroethylene synthesis kettle, pour the synthesis liquid into the synthesis kettle, wrap the heating jacket on the outside of the synthesis kettle, heat it up to 220°C, and keep heating at this temperature for 4 hours; The synthesized aluminum flakes were washed with deionized water, dried with high-pressure air, and then oven-dried at 60°C overnight. The obtained molecular sieve was confirmed to have an AEL structure by X-ray diffraction, but the compactness of the film was poor.

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Abstract

The invention discloses a method for ionothermal synthesis of aluminum phosphate AlPO4-n zeolite membranes under the condition that no organic or inorganic aluminum sources exist. The method for the ionothermal synthesis of the aluminum phosphate AlPO4-n zeolite membranes includes the steps: enabling precursor solution to be stirred for 1-10 hours under the condition of 80-100 DEG C to prepare synthesis solution, enabling a metal substrate to be put vertically into the synthesis solution, carrying out the ionothermal synthesis on the synthesis solution, taking out and cooling after the synthesis solution is through the ionothermal synthesis, using distilled water to washing the synthesis solution to be neutral, and drying to get the AlPO4-n zeolite membranes. The method for the ionothermal synthesis of the aluminum phosphate AlPO4-n zeolite membranes is simple and rapid. The zeolite membranes synthesized by the method is good in compactness, high in ducts of the zeolite membranes and capable of laying flatly on the surface of the substrate in orientation, preventing corrosive liquid from permeating the substrate from gaps or the ducts of the membranes and being strong in rotproofness.

Description

technical field [0001] The invention belongs to the field of synthesis and application of molecular sieve membranes, and in particular provides a rapid in-situ ion thermal synthesis of highly oriented AlPO without any organic or inorganic aluminum source precursor. 4 - A new approach to molecular sieve membranes. Background technique [0002] Corrosion is a natural phenomenon that pervades all fields of national economic construction. According to statistics, the annual economic loss caused by corrosion accounts for about 2-4% of the gross national product. Based on the estimation of my country's GDP of 33.5 trillion yuan in 2009, the economic loss caused by corrosion last year was at least as high as 670 billion yuan. For a long time, as a simple, economical and effective anti-corrosion method, anti-corrosion coatings have been widely used in various fields of the national economy, among which chromium-containing anti-corrosion coatings are the most widely used. However, ...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 蔡睿楚文玲杨维慎刘延纯俞同文
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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