NaY molecular sieve aggregate with nano-micro structure and preparation method thereof

A molecular and collective technology, applied in the field of molecular sieve preparation, can solve the problems of low product yield, mother liquor discharge, large template material, etc. Effect

Active Publication Date: 2018-11-23
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] To sum up, at present, the synthesis of mesostructured Y molecular sieves are all prepared by using water glass as raw material and modifying the synthetic gel in a hydrothermal system, and there are large template materials, low product yield, and mother liquor discharge. Quantity and other issues

Method used

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  • NaY molecular sieve aggregate with nano-micro structure and preparation method thereof
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  • NaY molecular sieve aggregate with nano-micro structure and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0069] The present embodiment provides a kind of preparation method of the NaY molecular sieve aggregate with nanostructure, it comprises the following steps:

[0070] 1) Take by weighing 57.81g water glass (SiO in water glass 2 The content is 28.08wt%, Na 2 The content of O is 8.83wt%) to be placed in the beaker, then take by weighing 8.81g sodium hydroxide solid (Beijing Century Hongxing Chemical Co., Ltd., analytically pure) and be placed in the beaker, the two are mixed and stirred evenly, and at room temperature (27 ℃) stirring for 2 hours to prepare a highly active hydrated sodium silicate solution;

[0071] Then add 54.11g deionized water, 3.12g sodium metaaluminate (Tianjin Jinke Chemical Research Institute, Al 2 O 3 The content is 45wt%, Na 2 The content of O is 41wt%), stirs and mixes evenly, adds 3g N in the system, N-dimethyl-N-hexadecylaminopropyl silane quaternary ammonium salt [(C n h 2n+1 O) 3 SiC 3 h 6 N(CH 3 ) 2 -C x h 2x+1 ]X, wherein, n=1; x=16...

Embodiment 2

[0079] The present embodiment provides a kind of preparation method of the NaY molecular sieve aggregate with nanostructure, it comprises the following steps:

[0080] 1) The preparation method and source of raw materials of the directing agent are the same as in Example 1.

[0081] 2) Weigh 32.54g of C-type silica gel (also known as coarse-porous microsphere silica gel) and add it to 50g of deionized water, then add 53.19g of water glass, and stir at a constant temperature of 20°C for 3 hours to prepare highly active hydrated silica gel. Then take by weighing the aluminum sulfate of 15.00g sodium metaaluminate and 17.64g (Tianjin Guangfu Technology Development Co., Ltd., Al 2 SO 4 18H 2 The O content is 99%) was dissolved in the highly active hydrated silica gel, and after stirring evenly, 83.38 g of the above-mentioned directing agent was added, and the reaction gel was obtained by stirring evenly.

[0082] 3) Put the above reaction gel into a stainless steel reaction ket...

Embodiment 3

[0085] The present embodiment provides a kind of preparation method of the NaY molecular sieve aggregate with nanostructure, it comprises the following steps:

[0086] 1) The preparation method and raw material sources of the directing agent are the same as in Example 1.

[0087] 2) Weigh 40.54g of coarse-porous microsphere silica gel and add it to 86g of deionized water, stir at a constant temperature of 20°C for 3 hours to prepare highly active hydrated silica gel, then weigh 20.00g of sodium metaaluminate into the highly active hydrated silica gel After stirring evenly, add 83.38g of the above-mentioned directing agent, and stir evenly to obtain a reaction gel.

[0088] 3) Put the above-mentioned reaction gel into a stainless steel reactor lined with tetrachlorethylene, statically crystallize at 100°C for 96 hours, then filter, wash and dry to obtain the NaY molecular sieve aggregate product.

[0089] The specific surface area of ​​the NaY molecular sieve aggregate product...

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Abstract

The invention provides a NaY molecular sieve aggregate with a nano-micro structure and a preparation method thereof. The method comprises the following steps of synthesizing a guide agent; preparing reaction gel by using the guide agent; performing crystallization on the reaction gel to obtain the NaY molecular sieve aggregate with the nano-micro structure, wherein organosilicon quaternary ammonium salt is introduced in the process of synthesizing the guide agent and/or preparing the reaction gel. The technical scheme provided by the invention has the advantages that the process is simple; thecost is low; the finally obtained product has a series of advantages of complete crystal phase, high silicon-aluminum ratio, high specific area, rich mesoporous-microporous structure, controllable crystal particle dimension and the like.

Description

technical field [0001] The invention relates to a NaY molecular sieve aggregate with nano-micro structure and a preparation method thereof, belonging to the technical field of molecular sieve preparation. Background technique [0002] Y-type molecular sieves are widely used in industry due to their special three-dimensional pore structure, high temperature stability and good catalytic activity. In the late 1950s, MILTON R.M. and BRECK D.W. (US3130007) successfully synthesized Y-type molecular sieves. Y-type molecular sieve replaces X-type zeolite as the main active component of the catalyst with its high stability, high activity, anti-metal pollution and anti-sintering ability. In the early 1970s, the American GRACE company (US 3639099, US 3671191) synthesized NaY molecular sieve by the directing agent method. The raw material was water glass instead of expensive silica sol, which simplified the process and shortened the production cycle, so that NaY molecular sieve was qui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/20
CPCC01B39/205C01P2002/60C01P2002/72C01P2004/03C01P2004/50C01P2004/51C01P2004/61C01P2006/12C01P2006/14
Inventor 巩雁军赵晓萌张恒蒙晓玲
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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