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A kind of synthetic method of β/y composite molecular sieve

A composite molecular sieve and a synthesis method technology, applied in the field of composite molecular sieve synthesis, can solve the problems of complex preparation method, high synthesis cost and high production cost of microporous composite molecular sieve, and achieve the advantages of simplified operation steps, improved yield and reduced energy consumption. Effect

Active Publication Date: 2011-12-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The microporous composite molecular sieve disclosed in this patent and its preparation method are complicated and the synthesis cost is relatively high
The disadvantage is that the β zeolite required in the second step needs to be synthesized by a specific method, and the β zeolite needs to be washed and dried to make Na-type β zeolite to synthesize the β / Y composite zeolite molecular sieve. The production cost in industrial production is relatively high

Method used

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  • A kind of synthetic method of β/y composite molecular sieve
  • A kind of synthetic method of β/y composite molecular sieve
  • A kind of synthetic method of β/y composite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 11.3g sodium hydroxide, 65mL distilled water, 5.8mL sodium aluminate solution (2.88mol / L), 33mL water glass (SiO 2 content 34wt%), shake vigorously, and age at 30° C. for 24 hours to obtain the Y structure directing agent.

[0040] Add 0.8g sodium hydroxide, 1.5mL sodium aluminate (2.88mol / L), 24g white carbon black, 100mL tetraethylammonium hydroxide (25wt%) to the beaker successively, stir for 3h, put the synthetic bomb in the oven Crystallize at 140°C for 5 hours to obtain β-seed crystals.

[0041] Add 100mL of distilled water, 4.6g of sodium hydroxide, 1.1mL of sodium aluminate (2.88mol / L), 12g of white carbon black, 6mL of β seed crystals into the beaker successively, stir for 30min, put the synthetic bomb into the oven for crystallization at 140°C 2d, the β molecular sieve slurry can be obtained.

[0042] Take 100mL of β molecular sieve slurry prepared in the previous step (the dry weight of β molecular sieve is about 4.6g), add 300mL of distilled water, 3mL...

Embodiment 2

[0049] Add 12.5g sodium hydroxide, 60mL distilled water, 5.8mL sodium aluminate solution (2.88mol / L), 31mL water glass (SiO 2 content 34wt%), shake vigorously, and age at 30° C. for 15 hours to obtain the Y structure-directing agent.

[0050] The preparation of the β molecular sieve slurry is the same as in Example 1. Add 220mL of distilled water, 2.3g of aluminum sulfate, and 0.2g of sodium hydroxide to 100mL of the β molecular sieve slurry (the dry weight of the β molecular sieve is about 4.6g), stir for 10min, and finally add 7mL of the Y structure directing agent, and stir After 30 minutes, put it into a synthetic bomb, and crystallize it in an oven at 120°C for 16 hours. The obtained product was washed with distilled water for 5 times to neutrality, and dried at 110° C. for 3 hours to obtain the β / Y composite molecular sieve. Wherein the weight content of the β molecular sieve in the composite molecular sieve is 59%.

Embodiment 3

[0052] Add 13g sodium hydroxide, 70mL distilled water, 4.5mL sodium aluminate solution (2.88mol / L), 30mL water glass (SiO 2 content 34wt%), shake vigorously, and age at 25°C for 24 hours to obtain the Y structure-directing agent.

[0053] The preparation of the β molecular sieve slurry is the same as in Example 1. Add 150mL of distilled water, 1.2g of aluminum chloride, and 1.5g of sodium hydroxide to 100mL of the β molecular sieve slurry (the dry weight of the β molecular sieve is about 4.6g), stir for 20min, and finally add 20mL of the Y structure directing agent, stir After 30 minutes, put it into a synthetic bomb, and crystallize it in an oven at 100°C for 30 hours. The obtained product was washed 4 times with distilled water to neutrality, and dried at 100° C. for 2 hours to obtain the β / Y composite molecular sieve. Wherein the weight content of the β molecular sieve in the composite molecular sieve is 49%.

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Abstract

The invention discloses an improved method for synthesizing a β / Y composite molecular sieve. It is characterized in that a two-step method is adopted: the first step is to prepare the Y structure-directing agent; the second step is to uniformly stir sodium hydroxide, water, aluminum source, β molecular sieve slurry and the Y structure-directing agent according to a certain mass ratio, and carry out The β / Y composite molecular sieve was prepared by crystallization. In the synthesis method provided by the present invention, the β molecular sieve precursor used is β molecular sieve slurry, and there is no need to wash and dry the β molecular sieve slurry to make Naβ molecular sieve or other β molecular sieves, which can save two-step unit operations. In this way, the silicon source and aluminum source that do not participate in the reaction in the β molecular sieve slurry can be fully utilized, and the yield of the composite molecular sieve is improved, thereby saving costs.

Description

technical field [0001] The invention relates to a method for synthesizing a composite molecular sieve. Specifically, it relates to a preparation method of a β / Y composite molecular sieve. Background technique [0002] β molecular sieve is currently the only macroporous high-silicon molecular sieve with intersecting twelve-membered ring channel system. Its skeleton structure is a symbiosis of tetragonal and monoclinic crystal systems, and three-dimensional twelve-membered ring channels are interlaced. β molecular sieves are widely used in many important reactions such as low-pressure hydrogenation, dewaxing, cracking, and isomerization of olefins or aromatics in the petrochemical industry. Y-type molecular sieves are one of the main varieties used as catalysts and adsorption separation agents. The catalysts made of Y-type molecular sieves are widely used in petroleum catalytic cracking and hydrocracking industries because of their high activity, good selectivity, and good st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24C01B39/46
Inventor 范峰张志智凌凤香张喜文孙万付沈智奇
Owner CHINA PETROLEUM & CHEM CORP