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Preparation method of hierarchical-pore CoAlPO-5 molecular sieve

A coalpo-5, multi-level pore technology, applied in the direction of molecular sieve and alkali exchange phosphate, can solve the problems of unfavorable molecular sieve synthesis mechanism, long crystallization time, etc., and achieve the effect of increasing crystallization rate and accelerating chemical reaction

Inactive Publication Date: 2014-05-28
LANZHOU UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

[0004] The purpose of the present invention is to provide a rapid synthesis method of multi-level pore CoAlPO-5 molecular sieves under atmospheric pressure, to overcome the disadvantages of long crystallization time in traditional synthesis and disadvantages of exploring the synthesis mechanism of molecular sieves under high temperature and pressure

Method used

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  • Preparation method of hierarchical-pore CoAlPO-5 molecular sieve
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  • Preparation method of hierarchical-pore CoAlPO-5 molecular sieve

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preparation example Construction

[0011] The present invention is the preparation method of hierarchical porous CoAlPO-5 molecular sieve, and its steps are:

[0012] (1) Mix succinic acid-choline chloride-tetraethylammonium bromide ternary eutectic mixture EM, aluminum isopropoxide and cobalt acetate tetrahydrate evenly, then add appropriate amount of phosphoric acid and hydrofluoric acid to obtain The mixed system is a: Co 2 o 3 ·Al 2 o 3 b:P 2 o 5 c: HF d: EM, where the coefficients are based on molar ratio: a = 0.2~0.6, b = 1.1~2.2, c = 0.45~1.35, d = 62.0~124.0, heated to 120 ℃ to make it evenly mixed, get a mixture;

[0013] (2) Heat the mixture to 175°C, and crystallize for 15 minutes under normal pressure or autogenous pressure;

[0014] (3) Cool the crystallized product to room temperature, repeatedly centrifuge and wash with water and acetone, and dry at 90 °C for 2 hours to obtain a powder product of hierarchically porous CoAlPO-5 molecular sieve.

[0015] According to the preparation method ...

Embodiment 1

[0023] (1) Mix and grind succinic acid, choline chloride, tetraethylammonium bromide, aluminum isopropoxide and cobalt acetate tetrahydrate evenly, transfer to a three-necked flask, and add appropriate amount of phosphoric acid and hydrofluoric acid with a pipette gun , the resulting mixture is a Co 2 o 3 ·Al 2 o 3 · b P 2 o 5 c HF d EM, where the coefficients are based on molar ratio: a = 0.4, b = 1.1, c = 0.45, d = 62.0, heated to a molten state (120 ℃) ​​with an electric heating mantle to make it evenly mixed;

[0024] (2) The above mixture was transferred to a microwave synthesizer, heated to 175 °C under microwave radiation, and crystallized under normal pressure or autogenous pressure for 15 minutes;

[0025] (3) Cool the obtained crystallized product to room temperature, repeatedly centrifuge and wash it with water and acetone, and dry it in a blast drying oven at 90 °C for 2 hours to obtain a powder product of heteroatom aluminum phosphate molecular sieve CoAlPO-5...

Embodiment 2

[0028] (1) Mix and grind succinic acid, choline chloride, tetraethylammonium bromide, aluminum isopropoxide and cobalt acetate tetrahydrate evenly, transfer to a three-necked flask, and add appropriate amount of phosphoric acid and hydrofluoric acid with a pipette gun , the resulting mixture is a Co 2 o 3 ·Al 2 o 3 · b P 2 o 5 c HF d EM, where the coefficients are based on molar ratio: a = 0.4, b = 1.1, c = 0.90, d = 62.0, heated to a molten state (120 ℃) ​​with an electric heating mantle to make it evenly mixed;

[0029] Steps (2), (3), and (4) are the same as in Example 1.

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Abstract

The invention relates to a preparation method of a hierarchical-pore CoAlPO-5 molecular sieve. The preparation method comprises the following steps: (1) uniformly mixing a succinic acid-choline chloride-tetraethylammonium bromide ternary eutectic mixture EM, aluminium isopropoxide and cobalt acetate tetrahydrate, then adding a proper amount of phosphoric acid and hydrofluoric acid so as to obtain a mixed system of a:Co2O3.Al2O3.b:P2O5.c:HF.d:EM, wherein coefficients are accounted in molar ratio that a is equal to 0.2-0.6, b is equal to 1.1-2.2, c is equal to 0.45-1.35 and d is equal to 62.0-124.0, and heating to 120 DEG C, so as to be mixed uniformly to obtain the mixture; (2) heating the mixture to 175 DEG C, carrying out crystallization for 15 minutes at an ordinary pressure or a self-generated pressure; (3) cooling the crystallization product to a room temperature, carrying out centrifugal washing repeatedly with water and acetone, and drying for 2 h at 90 DEG C so as to obtain a powder product of the hierarchical-pore CoAlPO-5 molecular sieve.

Description

technical field [0001] The invention relates to the preparation technology of molecular sieves. Background technique [0002] AlPO 4 -5 type molecular sieve [Al 12 P 12 o 48 ] is an aluminophosphate molecular sieve with AFI topology. This type of molecular sieve has a circular channel structure with twelve-membered rings, and its diameter is 7.3×7.3 nm. It belongs to the hexagonal system, and the unit cell size a = 1.38 nm , c = 0.86 nm. Due to AlPO 4 -5 has a neutral framework structure, the surface acidity is very weak, and there is almost no ion exchange performance, so the researchers introduced transition metals (such as Fe, Mn and Co, etc.) into AlPO through isomorphic substitution. 4 In the -5 molecular sieve, active centers separated from each other and highly dispersed were obtained. Moreover, the special pore structure of the molecular sieve provides a suitable space for the active center, so that it has both the oxidation active center and the selectivity t...

Claims

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Application Information

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IPC IPC(8): C01B39/54
Inventor 赵新红李晓斌陈静问娟娟祁永东赵江波
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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