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A kind of multi-component metal doped silicon phosphorus aluminum molecular sieve and its preparation method and application

A molecular sieve and metal technology, applied in the field of preparation of silicoaluminophosphate molecular sieve, can solve the problems of weak surface acidity and no ion exchange, and achieve the effects of improved hydrophobicity, excellent hydrophobicity and hydrothermal resistance, and low regeneration cost.

Active Publication Date: 2022-07-19
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 116g of phosphoric acid (85wt%) in 500g of water, then add 68g of pseudo-boehmite, 25g of 40wt% silica sol, constant temperature 40°C, and stir for 2 hours; then add 0.42g of ferrous sulfate heptahydrate, Add 25 g of copper acetate monohydrate, and continue to stir for 1 hour; then add 60 g of triethylamine, stir for 30 minutes; then add 36 g of diethylamine, add 20 g of Tmtac, and stir for 1 hour to obtain a gel mixture.

[0043] The gel mixture was transferred into a closed reactor, heated to 200°C for 2 hours, reacted at a constant temperature for 48 hours, cooled to room temperature, filtered, the obtained product was washed twice with deionized water, and dried at 120°C for 10 hours to obtain organic Molecular sieve powder of templating agent. The zeolite powder was heated to 550°C at a rate of 1°C / min for 4 hours in an air-circulating environment to obtain FeCu-silicon-phosphorus-aluminum molecular sieves.

[0044] N 2 Adsorption isotherm test BET spe...

Embodiment 2

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

[0049] The gel mixture was transferred into a closed reaction kettle, heated to 200°C for 2 hours, reacted at a constant temperature for 24 hours, cooled to room temperature, filtered, the obtained product was washed twice with deionized water, and dried at 120°C for 10 hours to obtain organic Molecular sieve powder of templating agent. The zeolite powder was heated to 550°C at a rate of 1°C / min for 4 hours in an air-circulating environment to obtain NiCu-silicophosphorus aluminum molecular sieves.

[0050] N 2 Adsorp...

Embodiment 3

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

[0055] The gel mixture was transferred into a closed reaction kettle, heated to 200°C for 2 hours, reacted at a constant temperature for 72 hours, cooled to room temperature, filtered, the obtained product was washed twice with deionized water, and dried at 120°C for 10 hours to obtain organic Molecular sieve powder of templating agent. The zeolite powder was heated to 550°C at a rate of 1°C / min and calcined for 4 hours in an air-circulating environment to obtain FeNiCu-silicon-phosphorus-alum...

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Abstract

The invention relates to a multi-element transition metal-doped metal silicoaluminophosphate molecular sieve and a preparation method thereof, wherein the metal atoms are at least two of vanadium, copper, molybdenum, cobalt, manganese, magnesium, iron, nickel and zinc, etc., And at least one of copper, iron and nickel is contained. The high-purity product was prepared by one-step hydrothermal reaction, and its anhydrous composition can be expressed as: mR·nMe·(Si x Al y P z )O 2 , where R is the template agent in the molecular sieve, m is per mole (Si x Al y P z )O 2 Contains the molar amount of the template agent, m=0.15-0.45; Me is the metal in the molecular sieve framework, and n is each mole (Si x Al y P z )O 2 The total molar amount of contained metals, n=0.01‑0.2, where each transition metal is relative to each mole (Si x Al y P z )O 2 The ratio is between 0.0001‑0.2. The synthesized metal silicoaluminophosphate molecular sieve has excellent adsorption performance, and the catalyst made from it can be applied to olefin synthesis and SCR denitration reaction.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve-type microporous material preparation and its application in catalytic process and mixed gas separation, in particular 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—aluminum phosphate molecular sieve AlPO4, which was an important milestone in the development of porous materials. This non-Si framework aluminum phosphate molecular sieve breaks the traditional idea that the molecular sieve is composed of silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron. However, AlO in AlPO4 molecular sieve 2- and PO 2 + The same number of tetrahedra results in the neutrality of the skeleton, weak surface acidity, and no ion exchange, which greatly limits its application. In 1984, U.S. Pat. No. 4,440...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/08C01B39/54B01J20/18B01D53/02B01D53/86B01D53/56B01J29/85C07C1/20C07C11/02
CPCC01B37/08C01B39/54B01J20/186B01D53/02B01D53/8628B01J29/85C07C1/20C01P2006/12C01P2006/16B01J2229/183C07C2529/85B01J35/617B01J35/615B01J35/643C07C11/02
Inventor 邵秘华赵宝刚宋成文孙涵孙玉清
Owner DALIAN MARITIME UNIVERSITY
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