Method for preparing high-stability mesoporous molecular sieve

A mesoporous molecular sieve, high stability technology, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of mesoporous structure, reduced interaction, high preparation cost, etc., to achieve high Molecular sieve yield, improve stability, reduce the effect of preparation cost

Active Publication Date: 2015-09-09
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The seed crystal selected in this invention is a microporous molecular sieve, which is added to the preparation system after silanization, and its hydrophobicity is used to increase its effect on the hydrophobic end of the surfactant micelle, thereby reducing the interaction between the two directing agents. However, the formed mesopores still do not have a regular structure, and whether the addition of seed crystals reduces the amount of templating agent has not been reported.
[0015] Bao X., et al, AIChE Journal.54 (7): 1850-1859 (2008) disclosed a preparation method for preparing micro-mesoporous molecular sieves. Specifically, the precursor of Y-type molecular sieves was prepared first, and P123 was used as a template for its preparation. Carry out assembly to prepare highly stable mesoporous molecular sieves, but the yield of mesoporous molecular sieves prepared by this method is only 2%, and the template agent required for preparing molecular sieves is 2g P123 / g molecular sieves, and its preparation cost is higher

Method used

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  • Method for preparing high-stability mesoporous molecular sieve
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Examples

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Embodiment 1

[0059] This embodiment provides a method for preparing a high-stability mesoporous molecular sieve, the method comprising the following steps:

[0060] (1), using Y-type molecular sieve precursor 1;

[0061] (2) Crystallization: Take 50g of Y-type molecular sieve precursor 1 solution, add 5g of seed crystals (meso-microporous molecular sieve prepared in Example 1 of CN201110101174.3) to assemble, adjust the pH value to 1, and stir at 30°C for 10 hours. After aging at 30°C for 20 hours, it was transferred to a crystallization tank, and after crystallization at 120°C for 24 hours, it was washed and dried to obtain JZ-1, a highly stable mesoporous molecular sieve. Its physical property is that the specific surface area is 678m 2 g -1 , Mesopore specific surface area 545m 2 g -1 , pore volume 1.08ml·g -1 , with an average pore size of 4.1nm.

Embodiment 2

[0063] This embodiment provides a method for preparing a high-stability mesoporous molecular sieve, the method comprising the following steps:

[0064] (1), using Y-type molecular sieve precursor 1;

[0065] (2) Crystallization: take 50g of the Y-type molecular sieve precursor 1 solution, add 10g of the product JZ-1 of Example 1 as a seed crystal for assembly, adjust the pH value to 1.2, stir at 20°C for 24 hours, and age at 50°C for 10h Move to a crystallization kettle, crystallize at 100°C for 48 hours, wash and dry to obtain high stability mesoporous molecular sieve JZ-2. Its physical property is a specific surface area of ​​656m 2 g -1 , Mesopore specific surface area 571m 2 g -1 , pore volume 1.01ml·g -1 , the average pore size is 3.9nm.

Embodiment 3

[0067] This embodiment provides a method for preparing a high-stability mesoporous molecular sieve, the method comprising the following steps:

[0068] (1), using Y-type molecular sieve precursor 1;

[0069] (2) Crystallization: Take 30g of the Y-type molecular sieve precursor 1 solution and add 2g of the product JZ-2 of Example 2 as a seed crystal for assembly, adjust the pH value to 1.5, stir at 50°C for 10 hours, and age at 20°C for 24h Move to a crystallization kettle, crystallize at 120°C for 24 hours, wash and dry to obtain high-stability mesoporous molecular sieve JZ-3. Its physical property is that the specific surface area is 612m 2 g -1 , Mesopore specific surface area 402m 2 g -1 , the pore volume is 1.13ml·g -1 , the average pore size is 5.1nm.

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Abstract

The invention provides a method for preparing a high-hydrothermal-stability mesoporous molecular sieve. The method includes the following steps: (1) preparation of a first Y-type molecular sieve precursor; and (2) crystallization: adding a seed crystal to the first Y-type molecular sieve precursor, adjusting the pH value to 0.5-5, stirring for 10 h-24 h at the temperature of 20 DEG C-50 DEG C, then aging for 2 h-24 h at the temperature of 20 DEG C-50 DEG C, to obtain an assembled product, transferring the assembled product into a microreactor with a polytetrafluoroethylene lining, then transferring together with the reactor into a high-pressure reaction kettle, crystallizing for 10 h-48 h at the temperature of 100 DEG C-200 DEG C, filtering, washing, drying, and thus obtaining the high-stability mesoporous molecular sieve. Firstly, the microporous molecular sieve precursor is prepared, a mesoporous-microporous molecular sieve as the seed crystal is used for preparation of the mesoporous molecular sieve, the molecular sieve precursor assembly method and the seed crystal method are combined, and the high-stability mesoporous molecular sieve is obtained under the condition without use of an organic template agent. Not only is the preparation cost of the molecular sieve reduced greatly, but also the process of calcination of the template agent is omitted so as to reduce the energy consumption.

Description

technical field [0001] The invention relates to a preparation method of a high-stability mesoporous molecular sieve, 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 towards industrial applications, reducing the preparation cost of mesoporous molecular sieves is the key to realizing the industrial application of mesoporous molecular sieves, and templates account for more than 70% of the pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24
Inventor 高雄厚刘洪涛赵晓争胡清勋刘宏海曹立刘超伟徐春艳张莉赵红娟王宝杰熊晓云王久江潘志爽田爱珍高永福王林曹庚振侯凯军
Owner PETROCHINA CO LTD
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