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A low-cost synthesis method of mesoporous molecular sieves

A technology of mesoporous molecular sieve and synthesis method, which is applied in the field of catalysts, can solve problems such as restricting industrial applications, and achieve the effect of long-range ordering

Active Publication Date: 2018-09-25
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0020] Using a suitable template system to assemble the precursor of microporous molecular sieves can greatly improve the acidity and stability of mesoporous molecular sieves, but the large amount of templates limits the industrial application of this technology

Method used

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  • A low-cost synthesis method of mesoporous molecular sieves
  • A low-cost synthesis method of mesoporous molecular sieves
  • A low-cost synthesis method of mesoporous molecular sieves

Examples

Experimental program
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Embodiment 1

[0065] The present embodiment provides a kind of synthetic method of mesoporous molecular sieve, comprises the following steps:

[0066] Step 1, using Y-type molecular sieve precursor 1;

[0067] Step 2, assembly: the concentration of 250g is 3% (EO) 20 (PO) 70 (EO) 20 (P123) solution was placed in a reaction vessel, placed in a water bath at 25°C, and 50g of Y-type molecular sieve precursor 1 was added dropwise under stirring. After the addition was completed, 1g of uncalcined micro-mesoporous molecular sieve was added as a seed crystal to adjust the pH 1, stirred for 2h, aged at 30°C for 20h to obtain the assembly product;

[0068] Step 3, crystallization: move the assembled product into a crystallization tank, crystallize at 120°C for 24 hours, filter, wash, dry, and calcine at 550°C for 10 hours to obtain mesoporous molecular sieve CS-1, which has a specific surface area of ​​711m 2 g -1 , Mesopore specific surface area 560m 2 g -1 , pore volume 1.09ml·g -1 , with ...

Embodiment 2

[0074] The present embodiment provides a kind of synthetic method of mesoporous molecular sieve, comprises the following steps:

[0075] Step 1, using Y-type molecular sieve precursor 2;

[0076] Step 2, assembly: the concentration of 250g is 3% (EO) 20 (PO) 70 (EO) 20 (P123) solution was placed in a reaction vessel, placed in a water bath at 25°C, and 50g of Y-type molecular sieve precursor 2 was added dropwise under stirring. After the addition was completed, 2g of uncalcined micro-mesoporous molecular sieve was added as a seed crystal to adjust the pH 1.5, stirred for 4h, aged at 30°C for 20h to obtain the assembled product;

[0077] Step 3, crystallization: move the assembled product into a crystallization pot, crystallize at 110°C for 48h, filter, wash, dry, and roast at 550°C for 10h to obtain mesoporous molecular sieve CS-2, whose physical property is a specific surface area of ​​728m 2 g -1 , Mesopore specific surface area 590m 2 g -1 , the pore volume is 1.19ml...

Embodiment 3

[0079] The present embodiment provides a kind of synthetic method of mesoporous molecular sieve, comprises the following steps:

[0080] Step 1, using Y-type molecular sieve precursor 3;

[0081] Step 2, assembly: the concentration of 200g is 4% (EO) 20 (PO) 70 (EO) 20 (P123) solution was placed in a reaction vessel, placed in a 25°C water bath, and 50g of Y-type molecular sieve precursor 3 was added dropwise under stirring. After the addition was completed, 3g of uncalcined micro-mesoporous molecular sieve was added as a seed crystal to adjust the pH was 0.75, stirred for 2 hours, and aged at 30°C for 20 hours to obtain the assembled product;

[0082] Step 3, crystallization: move the assembly product into a crystallization pot, crystallize at 150°C for 24h, filter, wash, dry, and calcine at 550°C for 10h to obtain mesoporous molecular sieve CS-3, whose physical property is a specific surface area of ​​687m 2 g -1 , Mesopore specific surface area 425m 2 g -1 , pore vol...

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Abstract

The invention provides a low-cost synthetic method of a mesoporous molecular sieve. In the method, a microporous molecular sieve precursor is synthesized firstly, and the precursor has the composition of (1-500)Na2O:Al2O3:(1-850)SiO2:(10-800)H2O; a segmented copolymer is adopted as a template agent and forms a synergistic effect with a microporous-mesoporous molecular sieve seed crystal under an acidic condition for assembling the precursor to obtain a mesoporous molecular sieve, and washing, filtration and roasting are carried out after crystallization to obtain the final product; in the process, the mesoporous molecular sieve can be synthesized in a low template agent system, and then the yield of the molecular sieve is substantially improved. The microporous-mesoporous seed crystal is used for synthesis of the mesoporous molecular sieve, the molecular sieve precursor assembly method and the seed crystal method are combined, the high-stability mesoporous molecular sieve can be obtained, and the yield of the mesoporous molecular sieve is relatively high; and at the same time, due to addition of the molecular sieve precursor and the seed crystal, the amount of the template agent is substantially reduced, and the cost is also reduced.

Description

technical field [0001] The invention relates to a low-cost synthesis method of mesoporous molecular sieves, belonging to the technical field of catalysts. Background technique [0002] Since mesoporous molecular sieves were first reported by the Moblil company of the United States in 1992, scholars at home and abroad have done a lot of work to improve their stability and acidity. For example, Zhao Dongyuan et al. used P123 as a template to collectively call a highly stable SBA-15 molecular sieve under acidic conditions, and Pinnavaia et al. used the method of assembling microporous molecular sieve precursors to greatly improve the acidity and stability of mesoporous molecular sieves. Although these works have pushed mesoporous molecular sieves toward industrial applications, reducing the synthesis cost of mesoporous molecular sieves is the key to truly realizing the industrial application of mesoporous molecular sieves, and templates account for more than 70% of the synthesi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24B01J29/08
Inventor 高雄厚刘洪涛胡清勋赵晓争刘宏海曹立刘超伟徐春艳熊晓云王宝杰赵红娟张莉王久江段宏昌田爱珍曹庚振王林侯凯军高永福
Owner PETROCHINA CO LTD