The synthetic method of small grain alpo4-34 aluminum phosphate molecular sieve

A technology of aluminum phosphate molecular sieve and synthesis method, applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve and alkali-exchanged phosphate and phosphorus compounds, etc., can solve the problem of large particle size of molecular sieve and the like

Active Publication Date: 2018-09-18
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] AlPO synthesized by the above patent 4 -34 grain size is greater than 5μm, the average particle size is about 8μm, and the molecular sieve particle size is still large

Method used

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  • The synthetic method of small grain alpo4-34 aluminum phosphate molecular sieve
  • The synthetic method of small grain alpo4-34 aluminum phosphate molecular sieve
  • The synthetic method of small grain alpo4-34 aluminum phosphate molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0042] At 20°C, 1.69g of pseudoboehmite (Al 2 o 3 content of 68%) was added to 20g of deionized water, stirred and mixed evenly, followed by adding 2.43g of morpholine, 1.02g of tetraethylammonium hydroxide (TEAOH content of 25%), stirring at 100°C for 12h and cooling down, adding 2.52 g orthophosphoric acid (H 3 PO 4 content of 85%), 0.5ml of hydrofluoric acid (HF content of 40%), stirred for 30 minutes, added 1.4g of AlPO4-34 seed crystals (particle size range 5-300nm), pre-crystallized at 100°C for 12h and then transferred to 25ml Crystallize at 190°C for 72 hours in a stainless steel reaction kettle lined with polytetrafluoroethylene, cool to room temperature, and centrifuge for solid-liquid separation. The solid product is washed with deionized water until neutral, collected, and dried in air at 80°C for 12 hours to obtain product. The grain size of the product is 0.05-0.6μm, and the average particle size is 0.4μm.

Embodiment 2

[0044] At 20°C, 1.69g of pseudoboehmite (Al 2 o 3 content of 68%) was added to 20g of deionized water, stirred and mixed evenly, followed by adding 2.90g of morpholine, 1.23g of tetraethylammonium hydroxide (TEAOH content of 25%), stirring at 100°C for 12h and cooling down, adding 2.52 g orthophosphoric acid (H 3 PO 4 content of 85%), 0.5ml of hydrofluoric acid (HF content of 40%), stirred for 30 minutes, added 1.5g of AlPO4-34 seed crystals (particle size range 5-300nm), pre-crystallized at 100°C for 12h and then transferred to 25ml Crystallize in a stainless steel reaction kettle at 190°C for 55 hours, centrifuge for solid-liquid separation, wash the solid product with deionized water until neutral, collect, and dry in air at 80°C for 12 hours to obtain the product. The grain size of the product is 0.1-0.9 μm, and the average particle size is 0.6 μm.

Embodiment 3

[0046] At 20°C, 1.69g of pseudoboehmite (Al 2 o 3 content of 68%) was added to 20g deionized water, after stirring and mixing evenly, 2.43g morpholine was added, stirred at 100°C for 12h, then cooled, and 2.52g orthophosphoric acid (H 3 PO 4 content is 85%), 0.5ml hydrofluoric acid (HF content is 40%), stirred for 30 minutes, added 1.4gAlPO 4 -34 seed crystals (particle size range 5-300nm), pre-crystallized at 100°C for 12h, then transferred to a 25ml stainless steel reactor for crystallization at 190°C for 72h, centrifuged for solid-liquid separation, and the solid product was washed with deionized water until neutral , collected, and dried in air at 80°C for 12 hours to obtain the product. The grain size of the product is 0.1-1μm, and the average particle size is 0.8μm.

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Abstract

The invention relates to a method for synthesizing small-crystal-grain aluminum phosphate molecular sieves AlPO4-34. According to the method, pseudo-boehmite or aluminum isopropoxide is used as an aluminum source, phosphoric acid serves as a phosphorus source, tetraethylammonium hydroxide and morpholine serve as template agents, and hydrofluoric acid serves as a fluorine source. The small-crystal-grain aluminum phosphate molecular sieves AlPO4-34, which are high in crystallinity and regular in crystal form, are synthesized by a pre-crystallization and seed crystal adding method on the basis of using the conventional raw materials and the mixed template agent. The grain size is small, and the average grain size is smaller than 1.5 microns and is only 0.05 to 1 micron after conditions are optimized. According to the method, the crystallinity is high, the morphology is regular, and the grain size distribution is uniform.

Description

technical field [0001] The invention relates to a small grain aluminum phosphate molecular sieve AlPO 4 Synthetic method of -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=0.90nm, b=0.93nm, c=0.95nm, and its structure 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 coordinations, and the Al-F bond will be broken at about 350°C, and the entire framework will transform into a CHA structure; at the same time, Al in the framework will strongly absorb water to form coordination, making the crystal form another a structure. Microporous aluminum phosphate molecular sieve AlPO 4 -34 has very good application prospects in water a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/04C01B39/54
CPCC01B37/04C01B39/54C01P2002/72C01P2004/03C01P2004/62C01P2004/64
Inventor 戴卫理杨柳曹戈李兰冬武光军关乃佳
Owner NANKAI UNIV
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