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Preparation method of polycrystal SAPO-53 molecular sieve

A SAPO-53, molecular sieve technology, applied in the direction of molecular sieve characteristic silicoaluminophosphate, molecular sieve and alkali-exchanged phosphate, etc., can solve the problems of preparation and use limitation, difficult synthesis, difficult synthesis, etc., and achieve low toxicity and strong irritation. and corrosive, stable effect

Inactive Publication Date: 2013-08-28
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the addition of Si source to AlPO 4 The synthesis of -53 molecular sieve has inhibitory effect, making SAPO-53 molecular sieve more than AlPO 4 -53 molecular sieves are more difficult to synthesize
In order to improve the acidity and acid strength of SAPO-53 molecular sieves, it is necessary to appropriately increase the silicon content. When methylamine is used as a template, the high silicon content makes the synthesis of SAPO-53 molecular sieves quite difficult, making the preparation of such molecular sieves and use is subject to certain restrictions

Method used

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  • Preparation method of polycrystal SAPO-53 molecular sieve
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  • Preparation method of polycrystal SAPO-53 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Weigh 30 grams of hexamethonium bromide into a round bottom flask, add 120 ml of absolute ethanol and 100 ml of isopropanol, then add 10 grams of sodium bromide and 20 grams of sodium hydroxide, and stir at 60°C for 4 to 6 hours. The reactant was cooled to room temperature, and sodium bromide was precipitated due to its low solubility in the alcoholic solution, and the hexanebiammonium hydroxide generated was dissolved in the alcoholic solution. After filtration, the filtrate was distilled under reduced pressure with a rotary evaporator to obtain hexanediammonium hydroxide with a yield of 91.2% and a purity of 85.6%. The evaporated organic solvent is recovered and reused.

[0032] Add 30ml of water to the beaker, add 7 grams of 65.5wt% pseudo-boehmite, drop 4ml of 85wt% phosphoric acid, after the pseudo-boehmite is completely dissolved, add 2.6 grams of hexanediammonium hydroxide, 30wt% silica sol 4ml, stirred for 1 hour to form a uniform silicoaluminophosphate gel, tr...

Embodiment 2

[0037] Weigh 30 grams of hexamethonium bromide into a round bottom flask, add 150 ml of absolute ethanol and 120 ml of isopropanol, then add 10 grams of sodium bromide and 25 grams of sodium hydroxide, and stir at 75°C for 4 to 6 hours. The reactant was cooled to room temperature, the precipitated sodium bromide was filtered, and the filtrate was distilled under reduced pressure at 20-70°C with a rotary evaporator to obtain hexanediammonium hydroxide with a yield of 89.1% and a purity of 84.8%. The evaporated organic solvent is recovered and reused.

[0038] Add 30ml of water to the beaker, add 8 grams of aluminum isopropoxide and 6 grams of hexanediammonium hydroxide in sequence, add 3ml of 85wt% phosphoric acid dropwise after dissolving, then add 8ml of 30wt% silica sol, and stir for 2 hours to form a uniform silica gel. The aluminum phosphate gel was transferred to a high-pressure reactor with a polytetrafluoroethylene liner, and was statically crystallized at 160°C for 2 d...

Embodiment 3

[0043] The specific steps and synthesis conditions are the same as in Example 1. The organic solvent used to prepare the template is a mixture of 150ml ethanol and 100ml n-propanol, the silicon source used is 2ml tetraethyl orthosilicate (TEOS), and the phosphorus source used is 2.5 grams of hydrogen phosphate Ammonium and 85wt% phosphoric acid 1.5ml, template agent hexane diammonium hydroxide dosage 3 grams, crystallization temperature 170 ° C, crystallization time 3 days.

[0044] Figure 5 is the XRD spectrum of the synthesized sample. It can be seen that the molecular sieve has an AEN structure and has a good crystallinity.

[0045] Image 6 This is the SEM image of the synthesized sample. Due to the low silicon content and relatively low temperature, the sample has a long strip-like stacked crystal appearance. There are glutinous rice-like crystal particles on the outer surface of the strip crystal, and the particle size is about 5-20 μm.

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Abstract

The invention relates to a preparation method of a polycrystal SAPO-53 molecular sieve, and the preparation method comprises the following steps of: adding hexamethonium bromide and alkali metal hydroxides to an organic solvent which contains a sedimentation promotor for ion exchange; filtering to remove sediments, and evaporating the organic solvent to obtain template agent hexane diammonium hydroxide; adding a silicon source, an aluminum source, a phosphorus source and the hexane diammonium hydroxide to water according to the mole ratio of SiO2:Al2O3:P2O5:R(OH)2:H2O=(0.1-15):1:(0.8-20):(0.3-25):(10-80), and stirring to form uniform gel; statically crystallizing at autogenous pressure inside a reaction kettle at 130-190 DEG C for 1-4 days; and filtering, washing and drying to obtain white SAPO-53 molecular sieve solid powder. The preparation method disclosed by the invention has the advantages of simplicity, easiness for operation and small usage amount of the template agent, greatly shortens the crystallization time, reduces the synthesis difficulty and production cost of a molecular sieve and can meet the particular requirement of different application occasions on the molecular sieve by controlling the appearance and particle diameter of a crystal by changing a reaction condition.

Description

technical field [0001] The invention relates to a method for synthesizing a silicoaluminophosphate molecular sieve, in particular to a method for preparing a microporous silicoaluminophosphate molecular sieve SAPO-53 with polycrystalline structure. Background technique [0002] Aluminum phosphate molecular sieve is a new type of molecular sieve (USP 4310440) developed by UCC in 1984 after the development of silicon aluminum molecular sieve. The characteristic of this type of molecular sieve is that the framework is composed of phosphorus-oxygen tetrahedrons and aluminum-oxygen tetrahedrons alternately linked, and the framework structure and pore structure are very rich. Molecular sieves containing only phosphorus and aluminum are not acidic due to the charge balance of the skeleton, so they have no catalytic performance. Therefore, the introduction of silicon and other metal heteroatoms into the formed silicoaluminophosphate molecular sieve (SAPO) and metalloaluminophosphat...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54
Inventor 武正簧石宝宝杨冬花张建英王新波冯晓娜李晓峰窦涛
Owner TAIYUAN UNIV OF TECH
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