Mesoporous IM-5 molecular sieve preparation method

A technology of IM-5 and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of diffusion product molecular sieve diffusion, decrease in reactivity and stability, unfavorable reactant molecules, etc., to achieve The effect of improving the anti-coking ability

Active Publication Date: 2017-08-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the small pore size (0.5-0.6nm) of mesoporous molecular sieves, the diffusion of some macromolecules into the pores is limited; Internal diffusion and product molecular sieve diffusion to the outer surface, which easily leads to a decrease in reactivity and stability

Method used

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  • Mesoporous IM-5 molecular sieve preparation method
  • Mesoporous IM-5 molecular sieve preparation method
  • Mesoporous IM-5 molecular sieve preparation method

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0056] (1) Preparation of IM-5 molecular sieve

[0057] IM-5 molecular sieves were synthesized by the method disclosed in the literature Synthesis, characterization, and catalytic properties of zeolites IM-5 and NU-88 (Journal of Catalysis 2003: 215151-170).

[0058] 3.00g (0.0075mol) of 1,5-bis(N-methylpyrrolidine) pentylene dibromide and 2.92g concentration of 50% NaOH aqueous solution, 0.427g Al(NO 3 ) 3 9H 2 O (98%, Junsei), 3.00g of white carbon black (Aerosil 200, Degussa) and 45.4g of deionized water were mixed to make a colloid, and the molar composition of the reaction mixture was SiO 2 :Al 2 o 3 : Na 2 O: SDA: H 2 O=1:0.0167:0.365:0.15:40, wherein SDA is 1,5-bis(N-methylpyrrolidine)pentylene dibromide.

[0059] The above mixture was stirred at 25°C for 30 minutes, then transferred to a closed crystallization kettle lined with polytetrafluoroethylene, and rotated and crystallized at 100 rpm and 160°C for 14 days. The crystallization reaction product was washed...

example 2

[0063] (1) Synthesize IM-5 molecular sieve according to the method of CN102452666A.

[0064] Dissolve 2.88g NaOH and 2.06g NaBr in 42.42g deionized water, add 0.17g NaAlO 2 Mix well with 16.02g of 1,5-bis(N-methylpyrrolidine)pentylene dibromide, and slowly add 40g of alkaline silica sol (SiO 2 The content is 30wt%, produced by Beijing Feilongma Science and Trade Co., Ltd., the pH value is 11.0), made into a colloid, and continued to stir 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.

[0065] The prepared colloid was transferred to a crystallization kettle lined with polytetrafluoroethylene, and rotated and crystallized at 160°C for 6 days. The crystallized reaction product was washed, filtered, and dried at 80°C for 12 hours to obtain IM-5 molecular sieve C. Its XRD spectrum shows that it is IM-5 molecular sieve with a crystallinity of 88.5%.

[0066] (2) Preparation of hydrogen-form IM-5 mol...

example 3

[0069] The following example prepares the mesoporous IM-5 molecular sieve of the present invention.

[0070] Dissolve 0.20g NaOH, 4.80g template agent 1,5-bis(N-methylpyrrolidine) pentylene dibromide in 16.20g deionized water, stir evenly, add 6g of IM prepared by the method of Example 1 and roasted -5 molecular sieves, mixed well, the molar composition of the reaction mixture is Z:B:R:H 2 O=1:0.05:0.12:9, wherein Z is the calcined IM-5 molecular sieve, B is the added alkali NaOH, and R is the template.

[0071] The above reactants were transferred to a 50ml autoclave lined with polytetrafluoroethylene, and subjected to dynamic crystallization treatment at 175°C for 3 hours. The processed product was washed with water, filtered, and dried at 80°C for 12 hours to obtain mesoporous IM-5 molecular sieves. Its crystallinity was 92.0%.

[0072] Mesoporous IM-5 molecular sieve is converted into hydrogen type by the method of example 1 (2) step, obtains hydrogen type mesoporous IM-...

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Abstract

The invention relates to a mesoporous IM-5 molecular sieve preparation method, which comprises: (1) dissolving an inorganic alkali or an organic alkali and a templating agent in water to prepare a mixed solution, and adding a microporous IM-5 molecular sieve to obtain a solid-liquid mixture, wherein a molar ratio of Z to B to R to H2O is 1:(0.01-0.03):(0.01-0.20):(5-40), Z is a microporous IM-5 molecular sieve (calculated as SiO2), the silicon oxide / alumina molar ratio of the microporous IM-5 molecular sieve is 40-200, B is an inorganic alkali or an organic alkali, R is a templating agent, the organic alkali is a quaternary ammonium alkali having a general formula NR14OH, and R1 is a C1-C2 alkyl or a 1,5-bis(N-methylpyrrolidine)pentane diquaternary ammonium alkali; and (2) carrying out hydrothermal crystallization treatment on the solid-liquid mixture obtained in the step (1) at a temperature of 120-200 DEG C, drying the solid obtained after the treatment, and calcining. According to the present invention, the prepared mesoporous IM-5 molecular sieve has intracrystal mesopores, and can provide high activity stability when the mesoporous IM-5 molecular sieve is used in toluene-methanol alkylation reactions.

Description

technical field [0001] The invention relates to a preparation method of a silica-alumina molecular sieve, in particular to a preparation method of a mesoporous IM-5 molecular sieve. Background technique [0002] The development of the petrochemical industry and the fine chemical industry, as well as the increasingly stringent requirements for sustainable development and environmentally friendly production, have led to an increasing demand for new catalytic materials. [0003] In 1997, French Petroleum Company (IFP) disclosed IM-5 molecular sieve for the first time in WO98 / 17581A1, CN1234012A. The molecular sieve has a two-dimensional ten-membered ring channel system and limited short channels in the third dimension. The channel system is very similar to the ZSM-5 molecular sieve and has good shape selectivity. At the same time, IM-5 molecular sieve has good thermal stability and hydrothermal stability, excellent catalytic performance, and has a wide range of applications in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/70
CPCB01J29/041B01J2229/14B01J2229/38C01B39/04C01P2002/72C01P2004/03
Inventor 陈俊文王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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