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Low-cost hierarchical pore SAPO-34 molecular sieve and preparation method and application thereof

A multi-stage pore, molecular sieve technology, applied in molecular sieve and alkali exchange phosphate, separation method, molecular sieve catalyst, etc., can solve the problem of high cost, achieve excellent low temperature activity, significant social and economic benefits.

Inactive Publication Date: 2020-09-15
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Aiming at the problem of high cost of the existing preparation method, the present invention uses lithium silicon powder waste as raw material to provide a preparation method of low-cost multi-stage porous SAPO-34 molecular sieve, which comprises the following steps:

Method used

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  • Low-cost hierarchical pore SAPO-34 molecular sieve and preparation method and application thereof
  • Low-cost hierarchical pore SAPO-34 molecular sieve and preparation method and application thereof
  • Low-cost hierarchical pore SAPO-34 molecular sieve and preparation method and application thereof

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preparation example Construction

[0034] Concrete, the preparation method of low-cost multi-stage porous SAPO-34 molecular sieve, it comprises the following steps:

[0035] A. Lithium silicon powder is washed with acid, dried and sieved to obtain powder;

[0036] B. Mix water and phosphorus source evenly to obtain phosphorus source solution;

[0037] C. Mix the powder obtained in step A with the phosphorus source solution obtained in step B, then add the templating agent under stirring, and mix evenly to obtain a mixed solution;

[0038] D. After the mixed solution obtained in step C is aged at room temperature, the temperature is raised to carry out hydrothermal crystallization to obtain a crystallization solution;

[0039] E. The crystallization solution obtained in step D is cooled, washed, filtered, dried and calcined to obtain low-cost multi-stage SAPO-34 molecular sieve.

[0040]Lithium silicon powder is a kind of industrial waste produced by the process of calcining spodumene at high temperature in th...

Embodiment 1

[0054] 4.16mLH 3 PO 4 Dissolve in 36mL deionized water, place on a magnetic stirrer and stir vigorously for 30min, add 3.34gAl 2 o 3 , continue to stir vigorously for 90 minutes, then slowly add 4 g of lithium silicon powder washed with 3 mol / L hydrochloric acid and dried through a 200-mesh sieve, stir for 60 minutes, then add 16.64 mL of template agent triethylamine, and stir vigorously for 90 minutes to form a uniform mixture. The mixed solution was filled into a polytetrafluoroethylene liner and sealed into a stainless steel reactor. After aging at room temperature for 12 hours, the temperature was raised to 200°C at a rate of 2°C / min and kept for 24h. After the reaction kettle is cooled, take out the mixed solution, wash it with deionized water until it is neutral, and dry it in an oven at 105°C for 12 hours to obtain the original powder of molecular sieve. ℃ in a tube furnace for 5 hours to remove the template agent, and the heating rate is 2 ℃ / min to obtain the SAPO-3...

Embodiment 2

[0056] 4.16mLH 3 PO 4 Dissolve in 36mL deionized water, place on a magnetic stirrer and stir vigorously for 30min, add 3.89gAl 2 o 3 , continue to stir vigorously for 90 minutes, then slowly add 1 g of lithium silica powder washed with 3 mol / L hydrochloric acid and dried through a 200-mesh sieve, stir for 60 minutes, then add 16.64 mL of template triethylamine, and stir vigorously for 90 minutes to form a uniform mixture. The mixed solution was filled into a polytetrafluoroethylene liner and sealed into a stainless steel reactor. After aging at room temperature for 12 hours, the temperature was raised to 200°C at a rate of 2°C / min and kept for 24h. After the reaction kettle is cooled, take out the mixed solution, wash it with deionized water until it is neutral, and dry it in an oven at 105°C for 12 hours to obtain the original powder of molecular sieve. ℃ in a tube furnace for 5 hours to remove the template agent, and the heating rate is 2 ℃ / min to obtain the SAPO-34 molec...

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Abstract

The invention discloses a low-cost hierarchical pore SAPO-34 molecular sieve and a preparation method and application thereof, and belongs to the technical field of molecular sieve synthesis. The invention provides preparation method of the SAPO-34 molecular sieve by taking lithium silicon powder waste as a raw material. The preparation method comprises the following steps: washing lithium siliconpowder with acid, drying and sieving to obtain powder; uniformly mixing water with a phosphorus source to obtain a phosphorus source solution; mixing the powder with a phosphorus source solution, adding a template agent, and uniformly mixing to obtain a mixed solution; aging the mixed solution at room temperature, heating, and carrying out hydrothermal crystallization to obtain a crystallizationsolution; and cooling, washing, filtering, drying and calcining the crystallization liquid to obtain the SAPO-34 molecular sieve. According to the invention, resource utilization is carried out on a large amount of waste residue lithium silicon powder piled up at present, and the SAPO-34 molecular sieve has a micro-mesoporous hierarchical pore structure by controlling the consumption of each material and optimizing the synthesis condition, so that the defect of a single microporous structure is effectively overcome, and the SAPO-34 molecular sieve can be used as a carrier material of a low-temperature denitration catalyst.

Description

technical field [0001] The invention belongs to the technical field of waste utilization and molecular sieve synthesis, in particular to a low-cost multi-stage porous SAPO-34 molecular sieve, a preparation method and application thereof. Background technique [0002] SAPO-34 molecular sieve has a typical CHA topology, and its skeleton is mainly composed of PO 2+ , AlO 2- , SiO 2 The tetrahedra are connected to each other, and these skeleton atoms are periodically arranged and combined into six-membered rings, four-membered rings and eight-membered rings, and finally form an ellipsoidal CHA cage structure and a three-dimensional cross-channel structure. SAPO-34 is actually Si atoms replacing AlPO 4 framework atoms are formed because in AlPO 4 Skeleton, PO 2+ and AlO 2- The tetrahedrons are positively charged and negatively charged respectively, and the number of the two is equal, so the entire skeleton is electrically neutral to the outside, and the surface acidity is v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D53/86B01D53/56B01J29/85C01B37/08C01B39/54
CPCB01D53/8625B01J29/85C01B37/08C01B39/54C01P2006/12C01P2006/16
Inventor 姚露蒋文举姚程杨林江霞
Owner SICHUAN UNIV
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