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Method of synthesizing IM-5 molecular sieve by using composite template

A composite template agent, IM-5 technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of IM-5 molecular sieve synthesis research, no related reports, unfavorable industrial scale-up, etc., to shorten the crystallization time and broaden the Proportion range, the effect of suppressing the formation of miscellaneous crystal phase

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

AI Technical Summary

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
[0005] 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 of synthesizing IM-5 molecular sieve by using composite template
  • Method of synthesizing IM-5 molecular sieve by using composite template
  • Method of synthesizing IM-5 molecular sieve by using composite template

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1 illustrates the effect of the IM-5 molecular sieve synthesis method provided by the present invention.

[0055] (1) Preparation of sodium metaaluminate (NaAlO 2 ) solution

[0056] Weigh 194g of NaOH and dissolve it in about 500ml of deionized water, add 153g of pseudo-boehmite (66.3% solid content), 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.

[0057] (2) Dissolve 2.95g NaOH in 20.65g deionized water, then add 4.01g NaAlO 2 Aqueous solution, 27.40g 1,5-bis(N-methylpyrrolidine) pentane bromide salt aqueous solution and 7.58g tetrapropylammonium bromide aqueous solution are mixed uniformly, under the condition of stirring, slowly dropwise add 40g alkaline silica sol, A gel was made and stirring was continued for 2 hours. The molar composition of the reaction mixture is: SiO 2 :Al 2 o 3 :Na 2 O:R1:R2:H 2 O=60:1:13.5:9:3:1200. Transfer the prep...

Embodiment 2

[0059] Example 2 illustrates the effect of the IM-5 molecular sieve synthesis method provided by the present invention.

[0060] 2.23g NaOH is dissolved in 15.63g deionized water, then add the NaAlO prepared by 6.02g embodiment 1 step (1) 2 Aqueous solution, 27.40g 1,5-bis(N-methylpyrrolidine) pentane bromide aqueous solution and 12.49g tetrapropyl ammonium hydroxide aqueous solution are mixed uniformly, under the condition of stirring, slowly dropwise add 40g alkaline silica sol, Then add SiO 2 The 5 wt% calcined IM-5 molecular sieve was used as a seed crystal 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:R1:R2:H 2 O=60:1.5:12:9:6:1200. 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 si...

Embodiment 3

[0062] Example 3 illustrates the effect of the IM-5 molecular sieve synthesis method provided by the present invention.

[0063] 4.48g NaOH is dissolved in 43.19g deionized water, then add the NaAlO prepared by 2.01g embodiment 1 step (1) 2 Aqueous solution, 36.54g 1,5-bis(N-methylpyrrolidine)pentane bromide salt aqueous solution and 22.74g tetrapropylammonium bromide aqueous solution are mixed uniformly, under the condition of stirring, slowly dropwise add 40g alkaline silica sol, A gel was made and stirring was continued for 2 hours. The molar composition of the reaction mixture is: SiO 2 :Al 2 o 3 :Na2O:R1:R2:H 2 O=60:0.5:18:12:9:1800. Transfer the obtained colloid to a 50ml polytetrafluoroethylene-lined autoclave, rotate and crystallize at 140°C for 7 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 provides a method of synthesizing IM-5 molecular sieve by using a composite template. The method comprises the following steps: (1) dissolving an inorganic base, an aluminum source and two templates in deionized water and carrying out uniform mixing so as to prepare a mixed solution; (2) adding a silicon source into the mixed solution obtained in step (1), optionally adding an additive and carrying out uniform mixing so as to prepare colloid or a solid-liquid mixture; (3) transferring the colloid or the solid-liquid mixture obtained in step (2) to a crystallization kettle, carrying out hydrothermal crystallization at a temperature of 120 to 200 DEG C for 1 to 10 d, carrying out cooling after crystallization and rinsing, filtering and drying the obtained mixed liquor so as to obtain raw powder of the IM-5 molecular sieve. A mole ratio of reactants satisfies the equation of SiO2: Al2O3: M2O: R1: R2: H2O = 60: 0.4-6: 6-21: 0.6-18: 0.6-12: 300-1800, wherein M2O is an alkali metal oxide, R1 is a first template, and R2 is a second template. The method provided in the invention widens the range of mixing ratios of raw materials, improves yield of a single kettle and enables time for crystallization to be further shortened and enlarged production to be easier.

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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Patent Type & Authority Applications(China)
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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