Double microporous-mesoporous composite molecular sieve and preparation method thereof

A composite molecular sieve and microporous technology, which is applied in molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve problems such as ternary dual microporous-mesoporous composite molecular sieves that have not been reported, and achieve large-scale industrial applications. value, the effect of good catalytic reactivity

Inactive Publication Date: 2011-05-04
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are many studies on binary microporous-mesoporous composite molecular sieves at home and abro

Method used

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  • Double microporous-mesoporous composite molecular sieve and preparation method thereof
  • Double microporous-mesoporous composite molecular sieve and preparation method thereof
  • Double microporous-mesoporous composite molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 0.47g Y-type and 0.47g Beta-type zeolite powders were mixed and pretreated and added to the mixed solution containing CTAB and OP-10, stirred at room temperature for 30min, then slowly added dropwise 5ml of water glass (SiO 2 25.4%, Na 2 O 7.4%), slowly add 0.389gAl after 5min 2 (SO 4 ) 3 18H 2 O, the raw material molar ratio is 1SiO 2 :0.15CTAB:0.025OP-10:x(Y+Beta):0.02Al 2 o 3 : 0.28Na 2 O: 60H 2 O, where (Y+Beta) / SiO 2 (mass ratio) = 0.53. After stirring for 1.0h, adjust the pH of the system to 11.1, continue to stir for 30min, put the glue into a lined reactor, and crystallize at 100°C for 48h. The product is suction filtered, washed, dried, and roasted. Ion exchange in 0.10mol / L ammonium nitrate solution at a ratio of 1:200 for 2.5h, suction filtration, drying, and finally roasting in the air to obtain an alkaline system. It is a 53% Y-Beta / MCM-41 double microporous-mesoporous composite molecular sieve, and this sample is named MYβ-1.

[0042] Depend o...

Embodiment 2

[0048] 0.47g Y-type and 0.47g Beta-type zeolite powders were mixed and pretreated and added to the mixed solution containing CTAB and OP-10, stirred at room temperature for 30min, then slowly added dropwise 5ml of water glass (SiO 2 25.4%, Na 2 O 7.4%), slowly add 0.156gAl after 5min 2 (SO 4 ) 3 18H 2 O, the raw material molar ratio is 1SiO 2 :0.15CTAB:0.025OP-10:x(Y+Beta):0.008Al 2 o 3 : 0.28Na 2 O: 60H 2 O, where (Y+Beta) / SiO 2 (mass ratio) = 0.53. After stirring for 1.0h, adjust the pH of the system to 11.1, continue to stir for 30min, put the glue into a lined reactor, and crystallize at 100°C for 48h. The product is filtered, washed, dried, and roasted. Ion exchange in 0.15mol / L ammonium chloride solution at a ratio of 1:300 for 2.0h, suction filtration, drying, and finally roasting in the air to obtain the Y-Beta / MCM with Si / Al=62.5 for the synthesis of alkaline system -41 double microporous-mesoporous composite molecular sieve, this sample is named MYβ-2.

Embodiment 3

[0050] 0.235g Y-type and 0.235g Beta-type zeolite powders were mixed and pretreated and added to the mixed solution containing CTAB and OP-10, stirred at room temperature for 30min, then slowly added dropwise 5ml of water glass (SiO 2 25.4%, Na 2 O 7.4%), slowly add 0.389gAl after 5min 2 (SO 4 ) 3 18H 2 O, the raw material molar ratio is 1SiO 2 :0.15CTAB:0.025OP-10:x(Y+Beta):0.02Al 2 o 3 : 0.28Na 2 O: 60H 2 O, where (Y+Beta) / SiO 2 (mass ratio) = 0.27. After stirring for 1.0h, adjust the pH of the system to 11.1, continue to stir for 30min, put the glue into a lined reactor, and crystallize at 100°C for 48h. The product is suction filtered, washed, dried, and roasted. Ion exchange in 0.10mol / L ammonium nitrate solution at a ratio of 1:200 for 2.5h, suction filtration, drying, and finally roasting in the air to obtain an alkaline system with a ratio of micropores of 1:1 and a relative content of 27% Y-Beta / MCM-41 double microporous-mesoporous composite molecular sieve...

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Abstract

The invention relates to a double microporous-mesoporous composite molecular sieve and a preparation method thereof. The molecular sieve is prepared by compounding Y and beta double microporous zeolites with an MCM-41 molecular sieve, and the wall of a hexagonal mesoporous phase is tightly coated by double microporous phases, so that a plurality of spherical or hemispherical empty shell structures are formed and interconnected to form a net, and the microporous phases have adjustable silicon-to-aluminum ratio and micropore content; and mixed liquid of hexadecyl trimethyl ammonium bromide and alkylphenol polyoxyethylene ether is taken as a template, pretreated silicon sources and/or aluminum sources of the double microporous phases and a synthesis mesoporous phase are introduced into a system respectively, and the Y-beta/MCM-41 double microporous-mesoporous composite molecular sieve which has the adjustable silicon-to-aluminum ratio and micropore content of the microporous phases is obtained through hydrothermal crystallization. The method is easy and convenient to operate, has high repeatability and is environmental-friendly; and by combining the advantages of the Y and beta zeolites and the mesoporous molecular sieve, the double microporous-mesoporous composite molecular sieve has high catalytic reaction performance and is used as a carrier material of a hydrocracking catalyst.

Description

technical field [0001] The invention relates to a catalyst carrier material composed of double microporous phase (Y type and Beta type zeolite) and mesoporous phase (MCM-41) molecular sieve and a preparation method thereof. Background technique [0002] As an important inorganic material, microporous molecular sieves are widely used as catalysts, adsorbents, ion exchangers and new functional materials due to their large specific surface area, high hydrothermal stability, uniform pore size, and adjustable surface properties. . The first industrial application of molecular sieves in the field of catalysis was the application of Y-type zeolite-based catalysts to isomerization by Union Carbide Corporation of the United States in 1959, followed by the application of X-type zeolites to catalytic cracking by American Mobile Corporation in 1962, and the application of X-type zeolite by Grace Corporation in 1969. The Ultrastable Y Zeolite (USY) catalyst was developed. At that time,...

Claims

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Application Information

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IPC IPC(8): B01J32/00B01J29/80B01J35/10C10G47/16
CPCC01B39/00C01B39/02
Inventor 王东青李全芝王刚张志华李旭光孙发民田然戴宝琴于春梅黄耀王甫村李海岩李井泉郭淑芝张庆武马守涛吕倩李淑杰孙生波李瑞峰
Owner PETROCHINA CO LTD
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