Multi-metal doped silicon-phosphorus-aluminum molecular sieve as well as preparation method and application thereof

A molecular sieve and metal technology, applied in the field of preparation of silicoaluminophosphate molecular sieve, can solve the problems of no ion exchange, weak surface acidity, etc., and achieve excellent hydrophobic and hydrothermal resistance, improved hydrophobicity, and improved hydrothermal stability. Effect

Active Publication Date: 2021-03-05
DALIAN MARITIME UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, AlO in AlPO4 molecular sieve 2- and PO 2 + The number of tetrahedrons is the same, resulting in an electrically neutral framework, weak surface acidity, and no ion exchange, which greatly limits its application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Slowly add phosphoric acid (85wt%) 116g in 500g water, then add pseudo-boehmite 68g, 40wt% silica sol 25g, constant temperature 40 ℃, after stirring 2 hours; Then add 0.42g ferrous sulfate heptahydrate, Add 25g of copper acetate monohydrate and continue to stir for 1 hour; then add 60g of triethylamine and stir for 30 minutes; then add 36g of diethylamine and 20g of Tmtac and stir for 1 hour to obtain a gel mixture.

[0043] Transfer the gel mixture into a closed reaction kettle, heat up to 200°C for 2 hours, react at a constant temperature for 48 hours, cool to room temperature, filter, wash the obtained product twice with deionized water, and dry at 120°C for 10 hours to obtain organic Molecular sieve powder for templating agent. The zeolite powder was heated up to 550°C at a rate of 1°C / min and calcined for 4 hours in an air-circulating environment to obtain FeCu-silicon-phosphorus-aluminum molecular sieves.

[0044] N 2 Adsorption isotherm test BET specific surfac...

Embodiment 2

[0048] Slowly add phosphoric acid (85wt%) 120g in 500g water, then add pseudoboehmite 75g, 40wt% silica sol 30g, constant temperature 40 ℃, after stirring for 2 hours; then add 24g nickel acetate tetrahydrate, add 15g Copper acetate monohydrate, continue to stir for 1 hour; then add 55 g of triethylamine, stir for 30 minutes; then add 36 g of diethylamine, add 20 g of tetraethylenepentamine, stir for 1 hour to obtain a gel mixture.

[0049] Transfer the gel mixture into a closed reaction kettle, heat up to 200°C for 2 hours, react at a constant temperature for 24 hours, cool to room temperature, filter, wash the obtained product twice with deionized water, and dry at 120°C for 10 hours to obtain organic Molecular sieve powder for templating agent. The zeolite powder was heated up to 550°C at a rate of 1°C / min and calcined for 4 hours in an air-circulating environment to obtain a NiCu-silicon-phosphorus-aluminum molecular sieve.

[0050] N 2 Adsorption isotherm test BET speci...

Embodiment 3

[0054] Slowly add phosphoric acid (85wt%) 120g in 500g water, then add pseudo-boehmite 75g, 40wt% silica sol 30g, constant temperature 40 ℃, stir after 2 hours; Then add 0.42g ferrous sulfate heptahydrate, Add 12g of nickel acetate tetrahydrate, add 25g of copper acetate monohydrate, and continue to stir for 1 hour; then add 60g of triethylamine, and stir for 30 minutes; then add 46g of diethylamine, add 20g of tetraethylenepentamine, and stir for 1 hour to obtain Gel mixture.

[0055] Transfer the gel mixture into a closed reaction kettle, heat up to 200°C for 2 hours, react at a constant temperature for 72 hours, cool to room temperature, filter, wash the obtained product twice with deionized water, and dry at 120°C for 10 hours to obtain organic Molecular sieve powder for templating agent. The zeolite powder was heated up to 550°C at a rate of 1°C / min and calcined for 4 hours in an air-circulating environment to obtain a FeNiCu-silicon-phosphorus-aluminum molecular sieve. ...

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Abstract

The invention relates to a multi-element transition metal doped metal silicoaluminophosphate molecular sieve and a preparation method thereof. Metal atoms are at least two of vanadium, copper, molybdenum, cobalt, manganese, magnesium, iron, nickel, zinc and the like, and at least contain one of copper, iron and nickel. A high-purity product is prepared through a one-step hydrothermal reaction method, the anhydrous composition of the high-purity product can be expressed as mR.nMe.(SixAlyPz)O2, wherein R is a template agent in the molecular sieve, m is the molar weight of the template agent contained in each mole of (SixAlyPz)O2, m is equal to 0.15-0.45, wherein Me is a metal in a molecular sieve skeleton, n is the total molar weight of metals contained in each mole of (SixAlyPz)O2, n is equal to 0.01-0.2, and the ratio of each transition metal to each mole of (SixAlyPz)O2 ranges from 0.0001-0.2. The synthesized metal silicoaluminophosphate molecular sieve has excellent adsorption performance, and a catalyst prepared from the metal silicoaluminophosphate molecular sieve can be applied to olefin synthesis and SCR denitration reaction.

Description

technical field [0001] The invention belongs to the technical field of preparation of molecular sieve-like microporous materials and their application in catalytic processes and separation of mixed gases, and specifically relates to the preparation and application of multi-element transition metal-doped silicoaluminophosphate molecular sieves. Background technique [0002] In 1982, scientists from United Carbide Corporation successfully synthesized a new molecular sieve—aluminophosphate molecular sieve AlPO4, which was an important milestone in the history of porous material development. This non-Si-skeleton aluminum phosphate molecular sieve breaks the traditional idea that molecular sieves consist of silicon-oxygen tetrahedrons and aluminum-oxygen tetrahedrons. However, AlO in AlPO4 molecular sieve 2- and PO 2 + The number of tetrahedrons is the same, resulting in an electrically neutral framework, weak surface acidity, and no ion exchange, which greatly limits its appl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B01J20/18B01D53/02B01D53/86B01D53/56B01J29/85C07C1/20C07C11/02
CPCC01B37/08C01B39/54B01J20/186B01D53/02B01D53/8628B01J29/85B01J35/1019B01J35/1023B01J35/1057C07C1/20C01P2006/12C01P2006/16B01J2229/183C07C2529/85C07C11/02
Inventor 邵秘华赵宝刚宋成文孙涵孙玉清
Owner DALIAN MARITIME UNIVERSITY
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