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Hydrothermal fluorine-free synthesis method of AlPO4-34

A synthetic method, hydrofluoric acid technology, applied in the direction of phosphorus compounds, molecular sieves and alkali-exchanged phosphates, molecular sieve characteristic aluminum phosphate, etc., can solve the problems of reduction, long crystallization time, waste of templates, etc., and achieve broad application prospects, The effect of implementing simple conditions

Inactive Publication Date: 2012-03-21
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A lot of expensive templates are wasted, the crystallization time is too long, there are defects such as miscellaneous crystals, which seriously reduce the reference value

Method used

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  • Hydrothermal fluorine-free synthesis method of AlPO4-34
  • Hydrothermal fluorine-free synthesis method of AlPO4-34
  • Hydrothermal fluorine-free synthesis method of AlPO4-34

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] At room temperature, take 10.00 milliliters of water and 1.74 grams of pseudo-boehmite (24.75% weight loss at 600°C) and stir and mix evenly, add 1.82 milliliters of phosphoric acid (85%) dropwise, stir and react evenly, and then pipette 2.96 milliliters of morpholine (analytically pure) was slowly added to the jelly, and stirred for half an hour. Transfer to a 20 ml stainless steel reaction kettle, and crystallize at 190° C. for 3 days under autogenous pressure. Quenching, washing, filtering, and natural drying to obtain the molecular sieve powder.

Embodiment 2

[0020] At room temperature, take 10 milliliters of water and 2.27 grams of aluminum isopropoxide (analytical pure) and stir and mix evenly, then pipette 1.97 milliliters of morpholine (analytical pure), slowly add to the above turbidity, stir and react evenly , 0.60 ml of phosphoric acid (85%) was added dropwise and stirred for half an hour. Transfer to a 20 ml stainless steel reaction kettle, and crystallize at 170° C. for 10 days under autogenous pressure. Quenching, washing, filtering, and natural drying to obtain AlPO 4 -34 molecular sieve raw powder.

Embodiment 3

[0022] At room temperature, take 10 milliliters of water and 1.74 grams of pseudo-boehmite (24.75% weight loss at 600°C) and stir and mix evenly, add 1.20 milliliters of phosphoric acid (85%) dropwise, stir and react evenly, and then pipette 3.95 milliliters of morpholine (analytically pure) was slowly added to the jelly, and stirred for half an hour. Transfer to a 20ml stainless steel reactor, and crystallize at 160°C for 15 days 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 relates to a method for synthetizing fluorine-free AlPO4-34 crystals with higher crystallinity and large grain size in proper treatment conditions, wherein hydrofluoric acid is not added, common organic amine morpholine (C4H9NO) is used as template agent, the traditional hydrothermal synthesis method is adopted and a proper raw material ratio is adopted. The method comprises the following steps: mixing aluminium source, phosphorus source, water and organic template agent evenly according to a certain molar ratio in sequence, wherein the molar ratio of Al2O3 to P2O5, R(morpholine) and H2O is 1.0:0.8-1.2:2.0-4.0:40-100; stirring to age, transferring the mixture in a stainless steel reaction kettle, crystallizing at 160-190 DEG C for 3-15 days under the generated pressure; then performing shock cooling, collecting, filtering, washing, and airing naturally to obtain AlPO4-34 molecular sieve raw powder. The method of the invention is green, environmentally friendly andeconomical, and has simple implementing conditions and wide application prospect.

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 common organic aminomorpholine (C 4 h 9 NO) as a template, using the traditional hydrothermal synthesis method to synthesize AlPO with high crystallinity and large grain size 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 microporous compounds. Among so many aluminum phosphate structures, AlPO 4 The -34...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/04C01B39/54
Inventor 李牛吴金雄项寿鹤
Owner NANKAI UNIV
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