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Method for synthesizing IM-5 molecular sieve

A technology of IM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of narrow synthesis range, difficult amplification, and narrow proportioning range, so as to shorten the crystallization time, shorten the synthesis time, and improve the single-pot Yield effect

Active Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When IM-5 molecular sieve is synthesized, the ratio range of raw materials is very narrow, especially when the ratio of sodium to silicon is only around 0.73, pure IM-5 molecular sieve can be synthesized, and a slight change will generate MOR, ZSM-12 and ANA and other miscellaneous crystal phases. The range is very narrow, which is not conducive to industrial amplification
The water content of the IM-5 molecular sieve synthesis system is too high, and the water-to-silicon ratio is not lower than 40, resulting in low single-pot yield, and it can only be synthesized in a small reaction pot (about 50ml), making it difficult to scale up
[0006] Due to less research on the synthesis of IM-5 molecular sieves, there is no relevant report so far to solve the above problems

Method used

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  • Method for synthesizing IM-5 molecular sieve
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  • Method for synthesizing IM-5 molecular sieve

Examples

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Embodiment 1

[0056] Example 1 illustrates the synthesis method of the IM-5 molecular sieve provided by the present invention.

[0057] (1) Sodium metaaluminate (NaAlO 2 ) solution preparation

[0058] Weigh 194g NaOH and dissolve in about 500ml deionized water, add 153g pseudo-boehmite (solid content 66.3%), and cook for 30min to obtain a clear and transparent solution. The obtained liquid was dubbed into 1L solution while it was hot, and cooled for later use.

[0059] (2) Dissolve 2.95g NaOH in 25.57g deionized water, then add 4.01g NaAlO prepared in step (1) 2 The aqueous solution and 27.40 g of 1,5-bis(N-methylpyrrolidine) pentane bromide salt solution were uniformly mixed, and under stirring, 40 g of alkaline silica sol was slowly added dropwise to form a colloid, and the stirring was continued for 2 hours. The molar composition of the reaction mixture is: SiO 2 :Al 2 o 3 :Na 2 O:R:H 2 O=60:1:13.5:9:1200, the ratio of water to silicon is 20:1. Transfer the prepared colloid to ...

Embodiment 2

[0061] Example 2 illustrates the synthesis method of the IM-5 molecular sieve provided by the present invention.

[0062] 1.65g NaOH is dissolved in 24.66g deionized water, then add the NaAlO prepared in 12.04g embodiment 1 step (1) 2 The aqueous solution and 18.27g of 1,5-bis(N-methylpyrrolidine)pentane bromide salt solution were mixed evenly, and under the condition of stirring, 40g of alkaline silica sol was slowly added dropwise, and then SiO 2 The calcined IM-5 molecular sieve with a weight of 5wt% was used as a seed crystal (seed) to make a colloid, and the stirring was continued for 2 hours. The molar composition of the reaction mixture is: SiO 2 :Al 2 o 3 :Na 2 O:R:H2O=60:3:13.5:6:1200, the ratio of water to silicon is 20:1. Transfer the prepared colloid to a 50ml polytetrafluoroethylene-lined autoclave, rotate and crystallize at 160°C for 5 days, stop the crystallization reaction, wash and filter the product, and dry it overnight at 80°C to obtain IM -5 molecula...

Embodiment 3

[0064] Example 3 illustrates the synthesis method of the IM-5 molecular sieve provided by the present invention.

[0065] Dissolve 2.88g NaOH and 2.06g NaBr in 21.95g deionized water, then add the 2.01g NaAlO prepared in Example 1 step (1) 2 The aqueous solution and 36.54g of 1,5-bis(N-methylpyrrolidine)pentane bromide salt solution were mixed evenly, and 40g of alkaline silica sol was slowly added dropwise under stirring to form a colloid, and the stirring was continued for 2 hours. The molar composition of the reaction mixture is: SiO 2 :Al 2 o 3 :Na 2 O:NaBr:R:H 2 O=60:0.5:12:6:12:1200, the ratio of water to silicon is 20:1. Transfer the obtained colloid to a 50ml polytetrafluoroethylene-lined autoclave, rotate and crystallize at 160°C for 4 days, stop the crystallization reaction, wash and filter the product, and dry it overnight at 80°C to obtain IM -5 molecular sieves.

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Abstract

The invention relates to a method for synthesizing IM-5 molecular sieve, which comprises the following steps: 1) dissolving inorganic base, aluminum source and a template in deionized water, uniformly mixing; 2) adding silicon source in a mixture obtained in the step 1), adding an additive or not to prepare colloid or a solid-liquid mixture, uniformly mixing; 3) moving the colloid or the solid-liquid mixture obtained in the step 2) to a crystallization kettle, carrying out hydrothermal dynamic crystallization at the temperature of 120-200 DEG C for 1-10 days, cooling after finishing the crystallization, washing the obtained mixed liquor, filtering and drying to obtain the IM-5 molecular sieve raw powder; wherein the mole ratio of the reactant is SiO2: Al2O3:M2O: R: H2O with 60: (0.3-6): (6-20): (0.6-18): (300-1800), M2O is alkali metal oxide and R is the template. The method of the invention has the advantages that IM-5 molecular sieve crystallization time is shortened, the raw material ratio range is wide, the single kettle yield is enhanced and the industrial amplification can be achieved.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, more specifically, a method for synthesizing IM-5 molecular sieves. Background technique [0002] Molecular sieves are playing an increasingly important role in the petrochemical industry. With the development of petrochemical and fine chemical industries, the requirements for environmental protection in the production process are becoming increasingly stringent, and the demand for new catalytic materials is also increasing. Among them, ten-membered ring molecular sieves are widely used in the field of shape-selective catalysis due to their unique pore size and pore structure. Only molecules whose size and shape match the pores of the molecular sieve can enter the pores of the molecular sieve. Using the difference in the size and structure of the pores of the molecular sieve, the "molecular sieve" can be realized to a certain extent, so that it has the ability of shape-selective cata...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 张超王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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