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A cobalt-based polymetallic single-atom isomorphously substituted phosphorus-aluminum molecular sieve meapo-5 and its preparation method

A phospho-aluminum molecular sieve and isomorphous substitution technology, which is applied in molecular sieve compounds, molecular sieve-specific aluminum phosphate, molecular sieve and alkali-exchanged phosphate, etc., can solve the problems of application limitation, lack of active sites of phospho-aluminum molecular sieve, etc., and achieves simple process operation. , Conducive to product diffusion, the effect of strong practicability

Active Publication Date: 2022-05-13
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the aluminum phosphorus molecular sieve itself lacks effective active sites, and its practical application in catalytic reactions is relatively limited.

Method used

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  • A cobalt-based polymetallic single-atom isomorphously substituted phosphorus-aluminum molecular sieve meapo-5 and its preparation method
  • A cobalt-based polymetallic single-atom isomorphously substituted phosphorus-aluminum molecular sieve meapo-5 and its preparation method
  • A cobalt-based polymetallic single-atom isomorphously substituted phosphorus-aluminum molecular sieve meapo-5 and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Mix pseudoboehmite, orthophosphoric acid, cobalt nitrate, yttrium nitrate, triethylamine, hydrofluoric acid and deionized water evenly, and the corresponding molar ratio is 1:1.31:0.08:0.009:0.75:0.05:30.00; The sequence is: 50% deionized water & phosphorus source - aluminum source - doped metal mixture - template agent. The preparation of the crystallization solution is as follows: take 30% deionized water and fully mix it with the calculated amount of hydrofluoric acid to form solution A; take another 20% deionized water, add the calculated amount of cobalt nitrate and yttrium nitrate, fully mix, and prepare It is solution B; under the condition of maintaining vigorous stirring, slowly drop solution B into solution A; fully stir until a uniform liquid mixture without precipitation is formed. During the preparation process, it is necessary to ensure that the temperature of the liquid is lower than 15°C; Slowly drop the mixture into the pre-mixed slurry of pseudo-boehmi...

Embodiment 2

[0041] Mix aluminum hydroxide, orthophosphoric acid, cobalt nitrate, tantalum nitrate, tri-n-propylamine, hydrofluoric acid and deionized water evenly, and the corresponding molar ratio is 1:1.21:0.05:0.01:0.5:0.01:43.00; crystallization The preparation of the solution is as follows: take 30% deionized water, fully mix it with the calculated amount of hydrofluoric acid, and make solution A; take another 20% deionized water, add the calculated amount of cobalt nitrate, mix it fully, and prepare it as solution B; Under the condition of maintaining vigorous stirring, slowly drop solution B into solution A; after that, add the calculated amount of tantalum nitrate, and stir fully until a uniform liquid mixture without precipitation is formed. During the preparation process, it is necessary to ensure that the liquid temperature is lower than 15 ℃; then slowly drop this liquid mixture into the slurry formed by the pre-mixing of aluminum hydroxide and orthophosphoric acid; then add th...

Embodiment 3

[0044] Mix SB powder, orthophosphoric acid, cobalt nitrate, zirconium nitrate, hafnium oxynitrate, (triethylamine + tri-n-propylamine), hydrofluoric acid and deionized water evenly, and the corresponding molar ratio is 1:1.57:0.01:0.01: 0.02: 0.5: 0.02: 28.00, the molar ratio of triethylamine to tri-n-propylamine is 0.42; the crystallization solution is prepared as follows: take 30% deionized water and fully mix it with the calculated amount of hydrofluoric acid to form solution A; Take 20% deionized water, add the calculated amount of cobalt nitrate and zirconium nitrate, mix thoroughly, and prepare solution B; under the condition of maintaining vigorous stirring, slowly drop solution B into solution A; after that, add the calculated amount Hafnium oxynitrate, fully stirred until a uniform liquid mixture without precipitation is formed. During the preparation process, it is necessary to ensure that the liquid temperature is lower than 15°C; then slowly drop this liquid mixture...

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Abstract

The invention provides a cobalt-based polymetallic single-atom isomorphously substituted phosphorus-aluminum molecular sieve MeAPO-5 and a preparation method thereof. The method uses aluminum source, phosphorus source, template agent, cobalt source, other doping metal sources and mineralizer as basic synthesis raw materials, and the maximum number of metal types that can be doped at the same time is 5. After fully mixing all the raw materials uniformly through a specific feeding sequence, the cobalt-based polymetallic single-atom MeAPO‑5 molecular sieve is prepared by two short-term crystallization methods. The process of the present invention is easy to operate, strong in practicability, and good in raw material compatibility. The prepared MeAPO-5 molecular sieve has high yield, many types of doped metals, high dispersion of metal sites, and the doped metals are in a single atomic state. The product has the characteristics of high particle size uniformity.

Description

technical field [0001] The invention relates to a cobalt-based polymetallic single-atom isomorphously substituted phosphorus-aluminum molecular sieve catalyst and a rapid preparation method thereof, belonging to the technical field of molecular sieve catalyst preparation. Background technique [0002] Aluminophosphate molecular sieves are aluminum phosphate molecular sieves without silicon and aluminum skeletons, and are new third-generation molecular sieves. Its basic structural unit is [PO 4 ] and [AlO 4 ] Oxygen-containing tetrahedra, the two are arranged alternately, and the orderly arrangement makes the internal pore structure stable, and has good thermal stability and reactivity. However, the aluminum phosphorus molecular sieve itself lacks effective active sites, and its practical application in catalytic reactions is relatively limited. [0003] In order to improve the catalytic performance of aluminum phosphorus molecular sieves, heteroatom molecular sieves have ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/06C01B39/54
CPCC01B37/065C01B39/54C01P2002/72C01P2004/03C01P2004/04
Inventor 邱宇刘东丑维超
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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