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Dynamically synthesized KL molecular sieve without structure-directing agent, and preparation method thereof

A synthesis method and technology of directing agent, applied in the field of molecular sieves, can solve the problems of increased synthesis cost and increased processing difficulty, achieve good purity and crystallinity, easy industrial scale-up, and simple synthesis method

Pending Publication Date: 2021-12-24
CHEM & CHEM ENG GUANGDONG LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the addition of structure-directing agents makes the post-processing of KL molecular sieve more difficult (such as the addition of organic alcohols requires high-temperature roasting to remove), and increases the synthesis cost

Method used

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  • Dynamically synthesized KL molecular sieve without structure-directing agent, and preparation method thereof
  • Dynamically synthesized KL molecular sieve without structure-directing agent, and preparation method thereof
  • Dynamically synthesized KL molecular sieve without structure-directing agent, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A non-zeolite structure directing agent KL dynamic synthesis method comprising the steps of: Weigh 19.52g KOH was dissolved in a small amount of water, followed by addition 4.50gAl (OH) 3 And heated to 100 deg.] C in a three-necked flask and stirred at reflux for 2h, Al (OH) 3 Complete dissolution, the solution is clear; until the solution was cooled to room temperature and transferred to a beaker, add the remaining water, stir, and then weighed 88.84g of silica sol (SiO 2 Content of 30wt.%) Was slowly added dropwise to the above solution, stirred at room temperature for 20 h aging, to obtain a sol-synthesized zeolite KL, the initial molar ratio of synthetic material to each sol 5.0K 2 O: 15.0SiO 2 : 1.0Al 2 O 3 : 292.65H 2 O. The above-synthesized sol was transferred to a PTFE lined 200mL, into a stainless steel crystallization autoclave, in a homogeneous reactor to speed 10r / min in 175 ℃ dynamic hydrothermal crystallization 24h, the resulting product was filtered off wi...

Embodiment 2

[0039] A non-zeolite structure directing agent KL dynamic synthesis method comprising the steps of: Weigh 21.47g KOH was dissolved in a small amount of water, followed by addition 4.50gAl (OH) 3 And heated to 100 deg.] C in a three-necked flask and stirred at reflux for 2h, Al (OH) 3 Complete dissolution, the solution is clear; until the solution was cooled to room temperature and transferred to a beaker, add the remaining water, stir, and then weighed 88.84g of silica sol (SiO 2 Content of 30wt.%) Was slowly added dropwise to the above solution, stirred at room temperature for 16 h aging, to obtain a sol-synthesized zeolite KL, the initial molar ratio of synthetic material to each sol 5.5K 2 O: 15.0SiO 2 : 1.0Al 2 O 3 : 292.65H 2 O. The above-synthesized sol was transferred to a PTFE lined 200mL, into a stainless steel crystallization autoclave, in a homogeneous reactor to speed 15r / min in 175 ℃ dynamic hydrothermal crystallization 24h, the resulting product was centrifuged to ...

Embodiment 3

[0044] A non-zeolite structure directing agent KL dynamic synthesis method comprising the steps of: Weigh 23.42g KOH was dissolved in a small amount of water, followed by addition 4.50gAl (OH) 3And heated to 100 deg.] C in a three-necked flask and stirred at reflux for 2h, Al (OH) 3 Complete dissolution, the solution is clear; until the solution was cooled to room temperature and transferred to a beaker, add the remaining water, stir, and then weighed 88.84g of silica sol (SiO 2 Content of 30wt.%) Was slowly added dropwise to the above solution, stirred at room temperature for 20 h aging, to obtain a sol-synthesized zeolite KL, the initial molar ratio of synthetic material to each sol 6.0K 2 O: 15.0SiO 2 : 1.0al 2 O 3 : 292.65H 2 O. The above-synthesized sol was transferred to a PTFE lined 200mL, into a stainless steel crystallization autoclave, in a homogeneous reactor to speed 15r / min in 175 ℃ dynamic hydrothermal crystallization 24h, the resulting product was filtered off wit...

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Abstract

The invention discloses a dynamically synthesized KL molecular sieve without a structure-directing agent, and a preparation method thereof. The preparation method comprises the following steps: mixing potassium hydroxide, an aluminum source, a silicon source and water according to a molar ratio of (4-7): 1: (12.0-18.0): (150-350), stirring and aging, crystallizing under a dynamic hydrothermal condition, and then separating, washing and drying to obtain the KL molecular sieve. Compared with other synthesis methods of the KL molecular sieve, the preparation method provided by the invention does not need to add an organic alcohol, seed crystal or metal ion structure directing agent, only needs to modulate the alkalinity and the silica-alumina ratio of the system, is simple, adopts dynamic synthesis conditions, and is easy for industrial amplification and large-scale batch production of the KL molecular sieve.

Description

Technical field [0001] Technical Field The present invention relates to molecular sieves, in particular, it relates to a process for its preparation KL zeolite structure directing agent-free dynamic synthesis. Background technique [0002] The topology is an LTL zeolite KL is conventional carriers basic catalyst aromatization of light hydrocarbons, developed first synthesized in 1965 by Union Carbide Corporation, having a one-dimensional 12-membered ring pore structure, pore size 0.71 nm, belonging to the hexagonal system (P6 / mmm, ), Having good hydrothermal stability, which is a noble metal Pt / KL catalysts exhibit excellent activity and selectivity of the aromatization reaction of light hydrocarbons aromatization, especially C5 ~ C8 straight-chain alkane aromatization reaction. [0003] KL zeolite main Synthesis by hydrothermal crystallization method, a silicon source, an aluminum source, a structure directing agent and water (seeds, templates, and metal ions, etc.) in a ...

Claims

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Application Information

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IPC IPC(8): C01B39/32
CPCC01B39/32C01P2002/72C01P2004/03C01P2004/30C01P2006/12
Inventor 陈会民李珂王苹王海丽丁湘浓王熙
Owner CHEM & CHEM ENG GUANGDONG LAB
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