Method for fluoride-free synthesis of AlPO4-34 from mixed solvents through hot process

A synthesis method and technology of hydrofluoric acid, applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali exchange phosphate, etc., to achieve the effect of broad application prospect, simple implementation conditions and high crystallinity

Inactive Publication Date: 2012-04-25
NANKAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, it is well known that AlPO can be synthesized without adding hydrofluoric acid 4 -34 is not an easy task

Method used

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  • Method for fluoride-free synthesis of AlPO4-34 from mixed solvents through hot process
  • Method for fluoride-free synthesis of AlPO4-34 from mixed solvents through hot process
  • Method for fluoride-free synthesis of AlPO4-34 from mixed solvents through hot process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] At room temperature, 6.60 milliliters of water was mixed with 1.74 grams of pseudo-boehmite (weight loss of 24.75% at 600° C.), and then 3.40 milliliters of isopropanol (analytical pure) was added, and stirred and mixed evenly. 1.20 ml of phosphoric acid (85%) was added dropwise, and the reaction was stirred evenly. Then, 1.97 ml of morpholine (analytical pure) was pipetted with a pipette, slowly added to the jelly, and stirred for half an hour. Transfer to a 25 ml stainless steel reactor, and crystallize at 170° C. for 6 days under autogenous pressure. Quenching, washing, filtering, and natural drying to obtain the molecular sieve powder.

Embodiment 2

[0020] At room temperature, take 2.50 milliliters of water and 1.74 grams of pseudo-boehmite (24.75% weight loss at 600° C.) and mix them, then add 7.50 milliliters of ethylene glycol (analytical grade), and stir and mix evenly. Add 1.20 milliliters of phosphoric acid ((85%) dropwise, stir and react evenly, then pipette 3.94 milliliters of morpholine (analytical pure), slowly add in the above-mentioned jelly, stir for half an hour. Transfer to 25 milliliters of stainless steel In the reaction kettle, crystallize at 185°C for 4 days under autogenous pressure. Quench, wash, filter, and dry naturally to obtain AlPO 4 -34 molecular sieve raw powder.

Embodiment 3

[0022] At room temperature, get 2.50 milliliters of water and mix with 0.87 gram of pseudo-boehmite (weight loss 24.75% at 600 DEG C), then add 7.50 milliliters of ethylene glycol (analytical pure), stir and mix well, add 0.91 milliliters of phosphoric acid (85 %), stir and react evenly, then pipette 3.94 milliliters of morpholine (analytical pure) and slowly add in the above-mentioned jelly, and stir for half an hour. Transfer to a 25 ml stainless steel reaction kettle, and crystallize at 200° C. for 1 day under autogenous pressure. Quenching, washing, filtering, and natural drying to obtain AlPO 4 -34 molecular sieve raw powder.

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Abstract

The invention mainly introduces a method for fast synthesizing high-crystallinity and high-yield fluoride-free AlPO4-34 through a mixed solvent hot process under the condition without hydrofluoric acid by using common organic amine morpholine as template agents and mixing isopropanol or ethylene glycol and water according to certain proportions. In the method, firstly, aluminum sources, phosphor sources, water, sopropanol or ethylene glycol and organic template agents are uniformly mixed in a certain sequence according to a certain mol rate that Al2O3/P2O5/morpholine/H2O/R (isopropanol or ethylene glycol)=1.0/0.8 to 1.2/2.0 to 8.0/12.5 to 75/4.0 to 24, the stirring and the ageing are carried out, the mixture is transferred into a stainless steel reaction kettle for being crystallized for 1 to 6 days at 170 to 200 DEG C at self generated pressure, then, sudden cooling, collection, filtering, washing and natural drying are carried out, and AlPO4-34 molecular sieve raw powder is obtained. The method has the advantages that green effect, environment protection and economy are realized, the implementation condition is simple, and wide application prospects are realized.

Description

technical field [0001] The invention relates to an aluminum phosphate molecular sieve AlPO 4 -34 synthesis methods. AlPO 4 The traditional synthesis methods of -34 are carried out under the highly toxic and highly corrosive HF medium, which seriously restricts its practical application and industrialization process. This patent mainly introduces the rapid synthesis of fluorine-free AlPO with high crystallinity and high yield by using common organic amines as templates and mixing isopropanol or ethylene glycol with water in a certain proportion as a mixed solvent without adding hydrofluoric acid. 4 Synthetic method of -34 crystal. 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 microporou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 李牛吴金雄项寿鹤
Owner NANKAI UNIV
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