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Synthetic method of AlPO4-34 aluminum phosphate molecular sieve

A technology of aluminum phosphate molecular sieve and synthesis method, which is applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve and alkali exchange phosphate, phosphorus compound, etc., which can solve the problems of high reactivity, unfavorable industrial production, low crystallinity, etc.

Inactive Publication Date: 2011-06-15
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As a template, piperidine has a strong pungent smell; the reactivity of aluminum hydroxide and aluminum oxide is not as high as pseudo-boehmite; the synthetic product using phosphoric acid as a phosphorus source has low crystallinity or needs to add a large amount of toxic Corrosive hydrofluoric acid helps increase crystallinity, which is not conducive to industrial production

Method used

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  • Synthetic method of AlPO4-34 aluminum phosphate molecular sieve
  • Synthetic method of AlPO4-34 aluminum phosphate molecular sieve
  • Synthetic method of AlPO4-34 aluminum phosphate molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] At 20°C, dissolve 0.46 g of phosphorous acid and 0.38 ml of phosphoric acid in 10 ml of water, pour the phosphorous acid aqueous solution into 0.87 g of pseudo-boehmite solid powder and stir, then add 0.2 ml of hydrofluoric acid, and drop while stirring Add 1.5 ml of morpholine, stir until uniform, then transfer to a 20 ml stainless steel reactor for crystallization at 200°C for 72 hours, then collect, wash and dry at 80°C according to the conventional post-treatment method of molecular sieves.

Embodiment 2

[0020] At 20°C, dissolve 0.64 g of phosphorous acid and 0.23 ml of phosphoric acid in 10 ml of water, pour the phosphorous acid aqueous solution into 0.87 g of pseudo-boehmite solid powder and stir, then add 0.2 ml of hydrofluoric acid, and drop while stirring Add 1.5 ml of morpholine, stir until uniform, then transfer to a 20 ml stainless steel reactor for crystallization at 200°C for 72 hours, then collect, wash and dry at 80°C according to the conventional post-treatment method of molecular sieves.

Embodiment 3

[0022] At 20°C, dissolve 0.27 g of phosphorous acid and 0.53 ml of phosphoric acid in 10 ml of water, pour the phosphorous acid aqueous solution into 0.87 g of pseudo-boehmite solid powder and stir, then add 0.2 ml of hydrofluoric acid, and drop while stirring Add 1.5 ml of morpholine, stir until uniform, then transfer to a 20 ml stainless steel reactor for crystallization at 200°C for 72 hours, then collect, wash and dry at 80°C according to the conventional post-treatment method of molecular sieves.

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Abstract

The invention provides a synthetic method of an AlPO4-34 aluminum phosphate molecular sieve. The method comprises the following steps of: by using phosphorous acid as phosphorus source or orthophosphorous acid-phosphoric acid as double phosphorus sources, pseudoboehmite as aluminum source and morpholine as template, according to the mole ratio of phosphorus source, aluminum source, organic template, hydrofluoric acid and water AlO2: H3PO3: Mor: HF: H2O of 0.5: 1.0: 0.5-3.0: 0.33-1.0: 25-200, or AlO2: H3PO3: Mor: HF: H2O of 0.5: 0.1-0.9: 0.5-3.0: 0.33-1.0: 25-200, preparing into a synthetic colloid; carrying out hydro-thermal crystallization on the colloid for 12-120 hours at the temperature of 160-200 DEG C and under self-generated pressure and then water washing; separating; keeping at the room temperature till the temperature of 80 DEG C to drying; and obtaining the product. Through the application of the method, the AlPO4-34 aluminum phosphate molecular sieve product with relatively higher purity and crystallinity can be prepared.

Description

technical field [0001] The present invention relates to the synthetic method of aluminum phosphate molecular sieve, specifically aluminum phosphate molecular sieve AlPO 4 Synthetic method of -34. AlPO with higher purity and crystallinity can be synthesized under the same conditions by using phosphorous acid instead of phosphoric acid as the phosphorus source or using phosphorous acid-phosphoric acid dual phosphorus source 4 -34. Background technique [0002] Aluminum phosphate molecular sieve AlPO 4 The skeleton of -34 is composed of P, Al, O, and F elements, and some Al and F form coordination, which belongs to the triclinic crystal system, and the unit cell size is a=0.90 nm, b=0.93 nm, c=0.95 nm. Similar to the CHA structure named by the International Zeolite Society, it has a cage-shaped pore system with an eight-membered ring opening. AlPO 4 In the framework of -34, part of Al and F form six-coordination, the Al-F bond will be broken at about 350°C, and the entire ...

Claims

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Application Information

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IPC IPC(8): C01B37/04C01B39/54
Inventor 李牛王晨光项寿鹤
Owner NANKAI UNIV