Preparation method of MCM-22 molecular sieve

A technology of MCM-22 and molecular sieve, which is applied in the field of preparation of MCM-22 molecular sieve, can solve problems such as long crystallization time and narrow range of silicon-aluminum ratio, so as to improve production efficiency, broaden the range of silicon-aluminum ratio, and shorten the crystallization reaction the effect of time

Active Publication Date: 2015-04-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] It can be seen from the above documents that although compared with the conventional hydrothermal method, the single-pot yield of MCM-22 molecular sieve prepared by the gas phase transfer method is higher and the environmental pollution is less, but there is still a relatively long crystallization time and the resulting product silicon aluminum Disadvantages of being narrower than

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  • Preparation method of MCM-22 molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take the original powder of MCM-22 (prepared by hydrothermal method, sodium type), the particle size is about 6 μm, SiO 2 / Al 2 O 3 The molar ratio is 20, according to the mass ratio H 2 The ratio of O / MCM-22=40, mix it with distilled water, and then disperse it with 20KHZ ultrasonic wave for 2 hours. Afterwards, the dispersed MCM-22 molecular sieve suspension was placed in a 100 mL measuring cylinder and allowed to settle naturally for 5 hours at room temperature. Take out the upper layer suspension, analyze the content of small grain MCM-22 molecular sieve and water in the suspension, and use it as a part of raw material, then according to SiO 2 / Al 2 O 3 =25、OH - / SiO 2 =0.12,H 2 O / SiO 2 =28 molar ratio, add the above suspension, sodium hydroxide, water, silicic acid, sodium aluminate to make initial sol, wherein the amount of suspension is 1.3% of the initial sol weight based on MCM-22 molecular sieve. When the sol formed a gel, the gel was aged at room te...

Embodiment 2

[0026] Prepare MCM-22 raw powder (hydrogen type) by hydrothermal method, the particle size is about 2 μm, SiO 2 / Al 2 O 3 The molar ratio is 30, according to the mass ratio H 2The ratio of O / MCM-22=70, mix it with distilled water, and then disperse it with 40KHZ ultrasonic wave for 1.5 hours. Afterwards, the dispersed MCM-22 molecular sieve suspension was placed in a 100 mL graduated cylinder at room temperature and allowed to settle naturally for 10 hours. Take out the upper layer suspension, analyze the content of small grain MCM-22 molecular sieve and water in the suspension, and use it as a part of raw material, then according to SiO 2 / Al 2 o 3 =40、OH - / SiO 2 =0.15,H 2 O / SiO 2 =30 molar ratio, add the suspension, sodium hydroxide, water, silica sol, and sodium aluminate to make the initial sol, wherein the amount of the suspension is calculated based on MCM-22 molecular sieve and accounts for 2.5% of the weight of the initial sol. After the sol forms a gel, th...

Embodiment 3

[0029] The sodium type small-grain MCM-22 raw powder prepared by the hydrothermal method has a particle size of about 700nm, and its SiO 2 / Al 2 o 3 The molar ratio is 30, according to the mass ratio H 2 The ratio of O / MCM-22=95, mix it with distilled water, and then disperse it with 80KHZ ultrasonic waves for 0.5 hours. Afterwards, the dispersed MCM-22 molecular sieve suspension was placed in a 100 mL graduated cylinder at room temperature and allowed to settle naturally for 15 hours. Take out the upper layer suspension, analyze the content of small grain MCM-22 molecular sieve and water in the suspension, and use it as a part of raw material, then according to SiO 2 / Al 2 o 3 =80,OH - / SiO 2 =0.17,H 2 O / SiO 2 = 40 molar ratio to add the suspension, sodium hydroxide, water, silicic acid, sodium aluminate to make the initial sol, wherein the amount of the suspension is calculated based on MCM-22 molecular sieve accounted for 4.8% of the weight of the initial sol. Af...

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Abstract

The invention discloses a preparation method of an MCM-22 molecular sieve, which adopts a vapor-phase transfer method. The method comprises the following steps: mixing MCM-22 molecular sieve powder and water to form a suspension, and carrying out ultrasonic dispersion treatment to peel out the small-grain MCM-22 molecular sieve; and by using the small-grain MCM-22 molecular sieve as the crystal seed, mixing with silicon source, aluminum source, alkali and water to prepare a silicon-aluminum xerogel. Due to the existence of abundant small-grain MCM-22 molecular sieve in the silicon-aluminum xerogel, the small-grain molecular sieve has the function of crystal seed in the MCM-22 molecular sieve preparation process by the vapor-phase transfer method, thereby obviously shortening the crystallization reaction time of the molecular sieve, enhancing the molecular sieve preparation efficiency, and widening the silicon-aluminum range of the MCM-22 molecular sieve synthesized by the vapor-phase transfer method to some extent under the induction crystallization of the crystal seed. The method has the advantage of simple preparation process, and is easy to implement.

Description

technical field [0001] The invention relates to a preparation method of MCM-22 molecular sieve, which belongs to the technical field of molecular sieve synthesis. Background technique [0002] MCM-22 molecular sieve is a kind of microporous crystalline molecular sieve, which has two sets of independent pore systems of ten-membered ring and twelve-membered ring. The dual channel system of MCM-22 molecular sieve makes it exhibit both the channel characteristics of ten-membered rings and the channel characteristics of twelve-membered rings in some catalytic reactions. At the same time, MCM-22 molecular sieve also has high thermal stability, hydrothermal stability and suitable acidity. Therefore, MCM-22 molecular sieves show high application value in alkylation, aromatization and toluene disproportionation. [0003] At present, most of the research on the synthesis of MCM-22 molecular sieves is the imitation or improvement of the earlier published patent USP 4954325 of Mobile ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
Inventor 杨卫亚沈智奇凌凤香王少军王丽华季洪海郭长友
Owner CHINA PETROLEUM & CHEM CORP
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