A kind of spherical heteroatom ni-sapo-34 molecular sieve and its preparation and application

A ni-sapo-34, heteroatom technology, applied in the direction of molecular sieve catalyst, molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, etc. Inexpensive and easy to obtain, the effect of facilitating transmission

Active Publication Date: 2019-03-19
SHANTOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of this invention is to provide a kind of preparation method of spherical heteroatom Ni-SAPO-34 molecular sieve, to solve the problem that the pressure drop of the catalyst bed is too large after the traditional cubic SAPO-34 molecular sieve is piled up, meanwhile, in SAPO-34 molecular sieve Ni elements are introduced into the framework structure to adjust the acid properties (acid type and acid strength) of molecular sieves and improve their catalytic performance

Method used

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  • A kind of spherical heteroatom ni-sapo-34 molecular sieve and its preparation and application
  • A kind of spherical heteroatom ni-sapo-34 molecular sieve and its preparation and application
  • A kind of spherical heteroatom ni-sapo-34 molecular sieve and its preparation and application

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Experimental program
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Effect test

Embodiment 1

[0030] Add 5ml of deionized water to 0.61g of nickel nitrate hexahydrate, the solution turns green after stirring, then add 0.452ml of diethylenetriamine solution, continue stirring, the solution turns from green to purple, and obtains Ni chelate solution A; Add 2.86g of aluminum isopropoxide, 1.05ml of phosphoric acid solution, 0.938ml of tetraethyl orthosilicate solution, and 2.07ml of morpholine solution into a 50ml glass beaker, then add 8.82ml of deionized water, 40 Stir for 6 hours under the condition of heating in a water bath at ℃, and the stirring speed is 350r / s to obtain the initial sol B; then add the Ni chelate solution A to the initial sol B, and continue to stir for 8 hours under the condition of heating in a water bath at 40°C to obtain sol C . The sol C was transferred into a reaction kettle lined with polytetrafluoroethylene, and after the filling was completed, the reaction kettle was moved into an oven for crystallization at 170° C. for 72 hours. After the...

Embodiment 2

[0032] Add 5ml of deionized water to 0.61g of nickel nitrate hexahydrate, the solution turns green after stirring, then add 0.452ml of diethylenetriamine solution, continue stirring, the solution turns from green to purple, and obtains Ni chelate solution A; Add 2.86g of aluminum isopropoxide, 1.05ml of phosphoric acid solution, 0.938ml of tetraethyl orthosilicate solution, and 2.07ml of morpholine solution into a 50ml glass beaker, then add 8.82ml of deionized water, 40 Stir for 4 hours under the heating condition of water bath at ℃, and the stirring speed is 400r / s to obtain the initial sol B; then add the Ni chelate solution A into the initial sol B, and continue stirring for 10 hours under the heating condition of the water bath at 40℃ to obtain the sol C . The sol C was transferred into a reaction kettle lined with polytetrafluoroethylene, and after filling the kettle, the reaction kettle was moved into an oven for crystallization at 190°C for 48 hours. After the crystal...

Embodiment 3

[0034] The steps in this embodiment are exactly the same as those in Embodiment 1. The difference is: in the raw material sampling and synthesis process, the added aluminum source is changed from 2.86g of aluminum isopropoxide to 1.02g of pseudo-boehmite. The prepared sample was analyzed as spherical heteroatom Ni-SAPO-34 molecular sieve.

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Abstract

The invention relates to a spherical heteroatom Ni-SAPO-34 molecular sieve, and a preparation method and an application thereof. The preparation method comprises the following synthesis steps: (1) dissolving nickel nitrate hexahydrate in deionized water, and dropwise adding a chelating agent at room temperature while stirring to obtain a Ni chelate solution A; (2) mixing an aluminum source, a phosphorous source, a silicon source, a template and deionized water, and heating and stirring the obtained mixture to obtain an initial sol B; (3) adding the solution A to the initial sol B, and heating and stirring the solution A and the initial sol B to obtain a sol C; and (4) filling a reaction kettle with the sol C, carrying out a crystallization reaction, filtering and washing a product obtained after the reaction is completed until the product is neutral, and drying, calcining and cooling the neutral product to obtain the spherical heteroatom Ni-SAPO-34 molecular sieve. The spherical heteroatom Ni-SAPO-34 molecular sieve with a high crystallinity is synthesized by a sol-hydrothermal synthesis technology, the pressure drop of an accumulated catalyst bed is effectively reduced, the introduction of metallic nickel provides many active sites for the reaction, and the molecular sieve has an important application in an NH3-SCR reaction. The synthesis method has the advantages of simple steps, and easiness in operation.

Description

technical field [0001] The invention belongs to the technical field of synthesis of heteroatom molecular sieves, in particular to a method for synthesizing spherical heteroatom Ni-SAPO-34 molecular sieves. Background technique [0002] Molecular sieves are silicon-phosphorus-aluminum molecular sieves with a CHA topology. Due to their unique pore structure, high specific surface area and moderate acidity, they are widely used in methanol-to-olefin, NH 3 - SCR catalytic reaction. In recent years, in order to improve the catalytic performance of SAPO-34 molecular sieve, many scientific researchers have carried out a series of modified synthesis on SAPO-34 molecular sieve. Among them, the modification of SAPO-34 by using metal ions has attracted extensive attention of researchers. [0003] Liu Hongxing and others used the method of solid-state ion exchange to modify SAPO-34. The analysis results showed that the acidity of SAPO-34 modified with CaO was reduced. Misook Kang syn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85
CPCB01J29/85B01J2229/183C01B37/08C01B39/54C01P2002/85C01P2004/03C01P2004/32C01P2004/61C01P2006/12
Inventor 方奕文张世超熊卫赵汝路旭朋陈文斌杨玲宋一兵
Owner SHANTOU UNIV
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