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Modified M-SAPO-RHO type zeolite molecular sieve and preparation method and applications thereof

A zeolite molecular sieve and modification technology, applied in the direction of molecular sieve and alkali exchange phosphate, separation methods, chemical instruments and methods, etc., can solve the problems of crystallinity decrease, achieve good repeatability, excellent adsorption and separation effect, cation type and The effect of adjustable content

Inactive Publication Date: 2020-04-10
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation method provided by the present invention does not need to remove the template agent before the ion exchange, and the obtained modified M-SAPO-RHO zeolite molecular sieve can overcome the problem of a large decrease in crystallinity in the traditional ion exchange process, and to a certain extent guarantees The stability of its structure; can effectively regulate the modified M-SAPO-RHO zeolite molecular sieve to CO 2 Excellent adsorption and separation effect, simple process

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  • Modified M-SAPO-RHO type zeolite molecular sieve and preparation method and applications thereof
  • Modified M-SAPO-RHO type zeolite molecular sieve and preparation method and applications thereof
  • Modified M-SAPO-RHO type zeolite molecular sieve and preparation method and applications thereof

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preparation example Construction

[0028] The invention provides a kind of preparation method of modified M-SAPO-RHO type zeolite molecular sieve, comprising the following steps:

[0029] Mixing a silicon source, an aluminum source, phosphoric acid, a template, cetyltrimethylammonium bromide, SAPO-RHO seed crystals and water to obtain an initial reaction gel; the template is diethylamine;

[0030] Crystallizing the initial reaction gel to obtain a SAPO-RHO type zeolite molecular sieve;

[0031] Mixing the SAPO-RHO type zeolite molecular sieve with a cationic solution, performing an ion exchange reaction and then roasting to obtain a modified M-SAPO-RHO type zeolite molecular sieve; the cations in the cationic solution include Na + 、K + and Cs + One or more of them; the concentration of the cationic solution is 0.2-1.0 mol / L.

[0032] In the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.

[0033]The invent...

Embodiment 1

[0067] Under the condition of stirring at room temperature, add 2.3g of phosphoric acid and 1.4g of pseudo-boehmite (oxidized 72wt%, the rest is crystal water) to 7mL of water, stir to make it evenly mixed, add 0.9g of silica sol and 0.1g of hexadecane Trimethylammonium bromide and stirred for 2 hours until uniformly mixed, then slowly added 1.75g ​​of diethylamine and stirred for 3 hours to obtain an initial gel, then added 0.036g of SAPO-RHO seed crystals and stirred for 15 minutes to obtain a uniform initial reaction gel; The sol was transferred into a high-pressure reactor, crystallized at 200°C for 48h, then filtered, and the resulting solid material was dried at 100°C for 12h to obtain DNL-6 zeolite molecular sieve (relative crystallinity: 100% , the purity is 100%, Si / (Si+Al+P) molar ratio=0.185).

[0068] XRD pattern of SAPO-RHO type zeolite molecular sieve figure 1 shown by figure 1 It can be seen that the synthetic product of the present invention is a SAPO-RHO typ...

Embodiment 2

[0072] According to the quality of the SAPO-RHO type zeolite molecular sieve and the ratio S / L=1:50 ratio of the cesium chloride solution volume, the SAPO-RHO type zeolite molecular sieve prepared in Example 1 and the 1mol / L cesium chloride solution were stirred at room temperature After mixing for 5 hours, filtering, washing the obtained solid material with deionized water, drying at 100°C for 12 hours, and then roasting in a muffle furnace at 600°C for 4 hours to obtain a modified Cs-SAPO-RHO zeolite molecular sieve; XRD spectrum as figure 1 As shown, the SEM image is shown in figure 2 As shown, the relative crystallinity is 75%, and the purity is 100%.

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Abstract

The invention provides a modified M-SAPO-RHO type zeolite molecular sieve and a preparation method and applications thereof, and belongs to the technical field of chemical engineering absorbents. Thepreparation method comprises following steps: mixing a silicon source, an aluminum source, phosphoric acid, a template, cetyl trimethyl ammonium bromide, a SAPO-RHO crystal seed, and water to obtain primary reaction gel, wherein the template is diethyl amine; crystallizing the primary reaction gel to obtain a SAPO-RHO type zeolite molecular sieve; directly mixing the SAPO-RHO type zeolite molecular sieve with a cationic solution without removing the template, carrying out ion exchange, and burning to obtain the modified M-SAPO-RHO type zeolite molecular sieve. The prepared modified M-SAPO-RHOtype zeolite molecular sieve has the advantages that the cation composition and content are controllable, the crystallization degree is high, and the performance on selectively adsorbing CO2 is strong.

Description

technical field [0001] The invention relates to the technical field of chemical adsorbents, in particular to a modified M-SAPO-RHO type zeolite molecular sieve and its preparation method and application. Background technique [0002] SAPO-RHO molecular sieves with RHO-type skeleton structure are widely used in the fields of gas adsorption separation, methanol to olefins and nitrogen oxide removal due to their advantages such as suitable pore volume, large specific surface area and adjustable acidity. . [0003] Tian et al. (Chem. Mater. 2011, 23, 1406-1413) used the denser SAPO-5 as a precursor and synthesized SAPO for the first time by phase transition under the condition of using diethylamine (DEA) as a template. - RHO molecular sieves. Su et al. (ChemSus Chem 2013, 6, 911-918) proposed a kind of SAPO xerogel as raw material, according to the molar ratio DEA:Al:P:Si:H 2 O molar ratio is 1.2:1:1:0.3:9.3 The new method of reacting the initial gel synthesis SAPO-RHO of rat...

Claims

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Application Information

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IPC IPC(8): C01B39/54B01J20/18B01J20/30B01D53/02
CPCB01D53/02B01D2257/504B01J20/186C01B39/54C01P2002/72C01P2004/03Y02P20/151Y02C20/40
Inventor 闫文付王晓贺白璞于吉红徐如人
Owner JILIN UNIV
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