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Aluminophosphate molecular sieve AlPO4-34 and fluoride-free preparation method thereof

A technology of aluminum phosphate molecular sieve and aluminum source, which is applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve and alkali-exchanged phosphate, phosphorus compound, etc., can solve problems such as uncontrollable interference, achieve good product crystallinity, simple and easy method, and high production efficiency high rate effect

Inactive Publication Date: 2015-03-25
天津神能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The problem to be solved in the present invention is to form AlPO without fluorine 4 The crystallization of -34 is very sensitive to the presence of water, and the interference of water in its structure formation cannot be controlled only under hydrothermal conditions, resulting in the formation of molecular sieves with other structures

Method used

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  • Aluminophosphate molecular sieve AlPO4-34 and fluoride-free preparation method thereof
  • Aluminophosphate molecular sieve AlPO4-34 and fluoride-free preparation method thereof
  • Aluminophosphate molecular sieve AlPO4-34 and fluoride-free preparation method thereof

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Embodiment 1

[0027] A kind of aluminum phosphate molecular sieve AlPO 4 The fluorine-free preparation method of -34 comprises the following steps:

[0028] At room temperature, mix 225ml of water with 135.5g of pseudo-boehmite, stir and mix well, then add 53.3ml of phosphoric acid dropwise, and stir for 2 hours to obtain a gel. The obtained gel was evaporated and concentrated at 60° C. for 4 hours to obtain a semi-dried gel, to which 174.2 ml of morpholine was slowly added dropwise, and stirred for 1.5 hours to obtain a synthetic colloid. Transfer it to a stainless steel reactor, and crystallize at 175° C. for 4 days under autogenous pressure. After quenching, collecting, filtering, washing, and drying naturally, the aluminum phosphate molecular sieve AlPO 4 -34.

Embodiment 2

[0030] A kind of aluminum phosphate molecular sieve AlPO 4 The fluorine-free preparation method of -34 comprises the following steps:

[0031] At room temperature, mix 270ml of water with 67.8g of pseudo-boehmite, stir evenly, add 33.3ml of phosphoric acid dropwise, and stir for 1.5h to obtain a gel. The obtained gel was evaporated and concentrated at 68° C. for 3 h to obtain a semi-dry gel. Slowly add 348.4ml of morpholine dropwise into the semi-dried gel, and stir for 1 hour to obtain a synthetic colloid. It was transferred to a stainless steel reactor, and crystallized at 180° C. for 3 days under autogenous pressure. After quenching, collecting, filtering, washing, and drying naturally, the aluminum phosphate molecular sieve AlPO 4 -34.

Embodiment 3

[0033] A kind of aluminum phosphate molecular sieve AlPO 4 The fluorine-free preparation method of -34 comprises the following steps:

[0034] At room temperature, mix 36ml of water with 40.8g of aluminum isopropoxide, stir evenly, add 7.3ml of phosphoric acid dropwise, and stir for 30 minutes to obtain a gel. The obtained gel was evaporated and concentrated at 50° C. for 1 hour to obtain a semi-dry gel, and 52.3 ml of morpholine was slowly added dropwise to the semi-dried gel, and stirred for 40 minutes to obtain a synthetic colloid. It was transferred to a stainless steel reactor, and crystallized at 185° C. for 1 day under autogenous pressure. After quenching, collecting, filtering, washing, and drying naturally, the aluminum phosphate molecular sieve AlPO 4 -34.

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Abstract

The invention provides an aluminophosphate molecular sieve AlPO4-34 and a fluoride-free preparation method thereof and belongs to the field of synthesis and preparation of molecular sieves. The fluoride-free preparation method of the aluminophosphate molecular sieve AlPO4-34 comprises steps as follows: firstly, evenly mixing an aluminum source, water and a phosphorus source to obtain gel, and evaporating and concentrating the gel to obtain half-dry gel; then adding an organic template to the obtained half-dry gel, and evenly strring the mixture to obtain synthetized gel, wherein the phosphorus source is phosphoric acid, and the organic template is morpholine. According to the fluoride-free preparation method of the aluminophosphate molecular sieve AlPO4-34, under the condition that no HF (hydrofluoric acid) is added, common organic amine is used as the template, the content of water in the gel is controlled through evaporation and concentration, and the aluminophosphate molecular sieve AlPO4-34 is synthetized with the high crystallinity and the high yield.

Description

technical field [0001] The invention relates to the technical field of synthesis and preparation of molecular sieves, in particular to an aluminum phosphate molecular sieve AlPO 4 -34 and its fluorine-free preparation method. Background technique [0002] It has been nearly 30 years since the discovery of aluminum phosphate molecular sieve in 1982. The aluminum phosphate molecular sieves found now have more than 53 structures, and most of these molecular sieves are small-pore, medium-pore, and macro-pore structures, and of course there are some ultra-large microporous compounds. Among so many aluminum phosphate structures, AlPO 4 The -34 is in a class of its own. [0003] AlPO 4 -34 has a chabazite-like structure, and the eight-membered ring has open channels. The skeleton is interlaced by double six-membered rings to form a cage structure. At the same time, 1 / 3 of Al in the framework adopts six-coordination, and adjacent six-coordinated Als are connected through F bri...

Claims

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Application Information

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IPC IPC(8): C01B37/04C01B39/54
CPCC01B37/04C01B39/54C01P2002/72C01P2004/03
Inventor 王震宇王宝义贾志远
Owner 天津神能科技有限公司
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