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Synthetic method of mesoporous-microporous molecular sieve by raising hydrothermal stability

A technology of microporous molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of inappropriate ratio of polymer and silicone modifier, small molecules, etc., and achieve the effect of long-term order preservation

Active Publication Date: 2012-10-24
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecular size of the silicone polymer they selected was small, or the ratio of the polymer to the silicone modifier was not suitable, and the molecular sieve did not produce a mesoporous structure.

Method used

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  • Synthetic method of mesoporous-microporous molecular sieve by raising hydrothermal stability
  • Synthetic method of mesoporous-microporous molecular sieve by raising hydrothermal stability
  • Synthetic method of mesoporous-microporous molecular sieve by raising hydrothermal stability

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Experimental program
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Effect test

preparation example Construction

[0066] Preparation of auxiliary templating agent 1:

[0067] 11 g of polypropyleneimine with a concentration of 50% and 1.0 g of vinyltrimethoxysilane were reacted at 50° C. for 12 hours to prepare auxiliary templating agent 1 .

[0068] Preparation of auxiliary templating agent 2:

[0069] 11 g of polyvinylamine with a concentration of 50% was reacted with 0.8 g of β-(3,4-epoxycyclohexyl)ethyltrimethoxysilane at 60° C. for 36 hours to prepare auxiliary templating agent 2 .

[0070] Preparation of auxiliary templating agent 3:

[0071] 20 g of polypropyleneimine with a concentration of 30% was reacted with 1.5 g of aminopropylaminoethyltrimethoxysilane at 100° C. for 12 hours to prepare auxiliary templating agent 3 .

[0072] Preparation of auxiliary templating agent 4:

[0073] 20 g of a 50% polyacrylamide solution was reacted with 1.5 g of 3-(2.3-glycidoxy)propyltrimethoxysilane at 50° C. for 36 hours to prepare auxiliary templating agent 4 .

[0074] Preparation of auxi...

Embodiment 1

[0089] Get 50g microporous molecular sieve precursor 1 solution and add in the reactor and be placed in 25 ℃ of water baths, the concentration of 200g is 5% (EO) 100 (PO) 70 (EO) 100 (F127) solution was added dropwise into the above system for assembly, adjusted the pH value to about 1, stirred for 10 hours after the dropwise addition, added 5g of auxiliary templating agent 1, stirred for 0.5h, and aged at 30°C for 15h. Transfer the product from the previous step to a crystallization kettle, crystallize at 120°C for 24 hours, filter and wash the crystallized product, dry it at 60°C for 24 hours, then transfer it to a muffle furnace, and roast it at 500°C for 6 hours to remove the template agent to obtain ultra-high water Thermally stable meso-microporous molecular sieve M-1.

Embodiment 2

[0091] Get 50g microporous molecular sieve precursor 2 solution and add in the reactor and be placed in 25 ℃ water bath, the concentration of 250g is 3% (EO) 100 (PO) 70 (EO) 100 (F127) solution was added dropwise into the above system for assembly, adjusted the pH value to about 5, stirred for 24 hours after the dropwise addition, added 5g of template aid 2, stirred for 0.5h, and aged at 30°C for 15h. Transfer the product from the previous step to a crystallization kettle, crystallize at 120°C for 24 hours, filter and wash the crystallized product, dry it at 90°C for 9 hours, then transfer it to a muffle furnace, and roast it at 700°C for 3 hours to remove the template agent to obtain ultra-high water Thermally stable meso-microporous molecular sieve M-2.

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Abstract

The invention relates to a synthetic method of a mesoporous-microporous molecular sieve, which is characterized in that a microporous molecular sieve precursor solution is synthesized, the precursor is composed of (1-500)Na2O: Al2O3: (1-850)SiO2: (10:800)H2O; a segmented copolymer is used as a main template, a modifier containing trimethoxy silane is used for modifying a polymer, the modified polymer is taken as an assisted template, an dual template is used for assembling the precursor solution of the microporous molecular sieve. According to the invention, the mesoporous-microporous molecular sieve presents great hydro-thermal stability and an adjustable tunnel structure, the specific surface area is between 800-1000m<2> / g, the hydrothermal treatment is carried out by 100% of water vapor with the temperature of 800 DEG C for 8 hours, the retention rate of the specific surface area can reach more than 39%, the hexagonal structure is still obvious, the long-distance ordered nature of the tunnel enables good preservation. The prepared catalyst presents good catalysis performance on the catalytic cracking of the heavy oil.

Description

technical field [0001] The invention relates to a method for synthesizing a meso-microporous molecular sieve, in particular to a method for synthesizing a meso-microporous molecular sieve with ultrahigh hydrothermal stability used as a heavy oil catalytic cracking catalyst. Background technique [0002] The availability of conventional petroleum resources is decreasing day by day, and the processing of heavy oil and residual oil is receiving more and more attention. Heavy oil is characterized by large molecules and complex molecular structures. Moreover, heavy oil is enriched with most of the sulfur, nitrogen and metal compounds in crude oil. These compounds are not only difficult to crack and easy to form coke, but also deposited on the surface of the catalyst are very easy to poison the catalyst and lose its activity. [0003] The above-mentioned characteristics of heavy oil put forward special requirements for catalytic cracking catalysts, and the existence of mesoporous...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 刘洪涛刘宏海高雄厚石永刚王坤赵红娟张莉王宝杰赵晓争熊晓云胡清勋
Owner PETROCHINA CO LTD
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