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Phosphate molecular sieve with afx structure and its preparation method

A phosphate and molecular sieve technology, applied in the field of phosphate molecular sieves and its preparation, can solve the problems of late research on the artificial synthesis of aluminum phosphate molecular sieves and no structure discovery

Active Publication Date: 2022-05-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Compared with zeolite molecular sieves, the artificial synthesis of aluminum phosphate molecular sieves is relatively late
In 1971, Flanigen et al. reported the synthesis of aluminum phosphate molecular sieves [Molecular Sieve Zeolites-I, ACS, Washington D.C]. Under hydrothermal synthesis conditions, mixed oxides of aluminum, silicon and phosphorus were obtained with analcime, chabazite, phillipsite -harmotome, L-type molecular sieve, A-type molecular sieve and B-type molecular sieve and other silicon-phosphorus-aluminum molecular sieves with the same crystal structure, wherein the content of phosphorus is 5-25% (as P2O5 ), but no structure different from zeolite molecular sieves was found

Method used

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  • Phosphate molecular sieve with afx structure and its preparation method
  • Phosphate molecular sieve with afx structure and its preparation method
  • Phosphate molecular sieve with afx structure and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Weigh 26 grams of N,N'-(1,4-phenylenebis(methylene))bis(N-methylmorpholine)ammonium hydroxide (hereinafter abbreviated as R) solution with a concentration of 15.74%, and then While stirring, add 0.698 g of pseudo-boehmite and 0.31 g of zinc acetate, then slowly drip 2.30 g of phosphoric acid solution with a concentration of 85%, and stir to obtain a synthetic mother liquor with the following molar ratios. :

[0035] 0.4ZnO:1.0Al 2 O 3 :2.4P 2 O 5 :3.6R:270H 2 O

[0036] The above-mentioned synthetic mother liquor was placed in a closed reaction vessel for crystallization, and the temperature was raised to 160 ° C at a temperature increase rate of 3 ° C / min. The crystallization time was 84 hours. After the crystallization product was washed and dried, a phosphate with AFX structure was obtained. Molecular sieves, such as figure 1 The XRD patterns shown and figure 2 The SEM image shown, the framework composition of the obtained phosphate molecular sieve is Zn 0....

Embodiment 2

[0038] Weigh 28.9 grams of N,N'-(1,4-phenylenebis(methylene))bis(N-methylmorpholine)ammonium hydroxide (hereinafter abbreviated as R) solution with a concentration of 15.74%, and then While stirring, add 0.698 g of pseudo-boehmite and 0.31 g of zinc acetate, then slowly drip 2.30 g of phosphoric acid solution with a concentration of 85%, and stir to obtain a synthetic mother liquor with the following molar ratios. :

[0039] 0.4ZnO:1.0Al 2 O 3 :2.4P 2 O 5 :4.0R:304H 2 O

[0040] The above-mentioned synthetic mother liquor was placed in a closed reaction vessel for crystallization, and the temperature was raised to 160° C. at a heating rate of 3° C. / min. The crystallization time was 60 hours. After the crystallization product was washed and dried, a phosphate with AFX structure was obtained. Molecular sieve, the skeleton composition of the obtained phosphate molecular sieve is Zn 0.09 Al 0.41 P 0.5 O 2 .

Embodiment 3

[0042] Weigh 14.4 grams of N,N'-(1,4-phenylenebis(methylene))bis(N-methylmorpholine)ammonium hydroxide (hereinafter abbreviated as R) solution with a concentration of 15.74%, and then While stirring, add 0.698 g of pseudo-boehmite and 0.31 g of zinc acetate, then slowly drip 2.30 g of phosphoric acid solution with a concentration of 85%, and stir to obtain a synthetic mother liquor with the following molar ratios. :

[0043] 0.4ZnO:1.0Al 2 O 3 :2.4P 2 O 5 :2.0R:152H 2 O

[0044] The above-mentioned synthetic mother liquor was placed in a closed reaction vessel for crystallization, and the temperature was raised to 170 ° C at a heating rate of 3 ° C / min, and the crystallization time was 72 hours. After the crystallization product was washed and dried, a phosphate with AFX structure was obtained. Molecular sieve, the skeleton composition of the obtained phosphate molecular sieve is Zn 0.07 Al 0.43 P 0.5 O 2 .

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Abstract

The present invention relates to a kind of zinc-containing phosphate molecular sieve with AFX structure and its preparation method, the skeleton of described molecular sieve has the composition of following molar ratio: (M a Si b al c P d )O 2 , where 0.01≤a≤0.2, 0≤b≤0.3, 0.3≤c<0.5, and a+b+c+d=1. The above-mentioned phosphate molecular sieve has the crystal structure of AFX, and this structure can still be kept stable under the condition of high temperature treatment, so it can be used as an adsorbent, and can also be used as a catalyst or a catalyst carrier.

Description

technical field [0001] The present invention relates to a phosphate molecular sieve and a preparation method thereof. Background technique [0002] Molecular sieve is a porous crystalline material with large specific surface area and open internal space, which can be used to accommodate some guest molecules, such as metals, metal oxides, organic molecules, water molecules, etc., and can also be used as where the catalytic reaction takes place. Since molecular sieves have uniform and regular pores, and the pore size is of the same order of magnitude as the molecules, it is possible to "select" the entry and exit of the molecules, thereby obtaining the shape-selective effect. Because molecular sieves have the above characteristics, they are widely used as catalysts, catalyst carriers, adsorbents and detergents, etc., and have been widely used in petrochemical, environmental protection, and adsorption and separation fields. The framework of molecular sieves is usually compose...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/85
CPCC01B37/065C01B37/08C01B39/54B01J20/18B01J20/0292B01J29/84B01J29/85C01P2002/72C01P2004/03Y02P20/52
Inventor 袁志庆付文华刘松霖
Owner CHINA PETROLEUM & CHEM CORP
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