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Nano ZSM-5 molecular sieve based catalyst and preparation and use methods

A technology of ZSM-5 and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve the effect of improving the overall aromatics selectivity, wide range of applicable raw materials, and reducing the production rate

Active Publication Date: 2015-09-30
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The acidic strength and acid site distribution of ZSM-5 will also have a huge impact on its catalytic performance. Studies have shown that lower Si / Al can improve the selectivity of aromatics, and at the same time generate a large amount of light hydrocarbons, and the selectivity of aromatics cannot exceed 80%. , strong acids are prone to hydrogen transfer to light hydrocarbons

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the preparation method of molecular sieve catalyst comprises the following steps:

[0031] Step 1: 2g of silica sol, 0.02g of aluminum nitrate, 0.36g of TPAOH (25% aqueous solution), 2g of urea, 0.1g of isopropanol, 18g of water were mixed and stirred at room temperature to form a precursor aqueous solution, and then the precursor aqueous solution was transferred to Put it into a synthesis kettle, seal it, and crystallize it at 120°C for 72h. After the crystallization, separate the reaction mixture from solid to liquid, wash it with deionized water, dry the solid at 90°C for 3h, and finally bake it in an air atmosphere at 450°C for 1h. , to obtain molecular sieve raw powder, the raw powder particle size is 1 ~ 2 μm × 500nm ~ 1 μm × 3 ~ 3.5 μm ([100] direction (a axis) × [010] direction (b axis) × [001] direction (c axis) );

[0032] Step 2: Mix and stir the molecular sieve powder with 20 mL of 0.1 mol / L ammonium salt solution for 1 h, filter, and mix the ...

Embodiment 2

[0035] Embodiment 2: the preparation method of molecular sieve catalyst comprises the following steps:

[0036] Step 1: 21g of silica sol, 3.6g of aluminum nitrate, 32.4g of TPAOH (25% aqueous solution), 17g of urea, 9g of isopropanol, 18g of water, mixed and stirred at room temperature to form a precursor aqueous solution, and then the precursor aqueous solution was transferred to In the synthesis kettle, seal it, and crystallize it at 120°C for 72h. After the crystallization, separate the reaction mixture from solid to liquid, wash it with deionized water, dry the solid at 90°C for 3h, and finally bake it in an air atmosphere at 650°C for 10h. Get molecular sieve raw powder, raw powder particle size is 1~2μm×500nm~1μm×3~3.5μm ([100] direction (a axis)×[010] direction (b axis)×[001] direction (c axis)) ;

[0037] Step 2: Mix and stir the molecular sieve raw powder with 20 mL of 0.1mol / L ammonium salt solution for 24 hours, filter, and mix and stir the filter cake with 0.1mol...

Embodiment 3

[0040] Embodiment 3: the preparation method of molecular sieve catalyst comprises the following steps:

[0041] Step 1: Mix and stir 11g TEOS, 0.3g aluminum nitrate, 18g TPAOH,,, 2g urea, 0.2g KOH, and 18g water at room temperature to prepare a precursor aqueous solution, then transfer the precursor aqueous solution into a synthesis kettle, seal it, Crystallize at 180°C for 48h. After crystallization, the reaction mixture is separated from solid and liquid, washed with deionized water, dried at 90°C for 24h, and finally calcined in an air atmosphere at 550°C for 10h to obtain a molecular sieve powder with a size of 400~500nm×150nm~200nm×2μm~2.5μm ([100] direction (a axis)×[010] direction (b axis)×[001] direction (c axis)).

[0042] Step 2: Mix and stir the molecular sieve raw powder with 20 mL of 0.1mol / L ammonium salt solution for 24 hours, filter, and mix and stir the filter cake with 0.1mol / L ammonium salt solution for 24 hours again, filter, and repeat this 5 times, at 100...

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PUM

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Abstract

The invention discloses a nano ZSM-5 molecular sieve based catalyst and preparation and use methods. The molecular sieve catalyst consists of molecular sieves and metal components, wherein the molecular sieves are nano ZSM-5 molecular sieves with a short b-axis, a medium high silica-alumina ratio, less strong acid, high Lewis acid content, and resistance to hydrothermal deactivation. The preparation method is as follows: mixing a silicon source, an aluminum source, a template agent, a structure promoter, an additive and alkali with water, and stirring to prepare a precursor solution, then crystallizing, separating solid from liquid, and calcinating to obtain molecular sieve raw powder; mixing the molecular sieve raw powder with an ammonium salt solution, stirring, filtering, mixing with the ammonium salt solution for several times, stirring, filtering, and calcinating to obtain hydrogen-type ZSM-5 molecular sieves; mixing with the metal precursor solution, drying and calcinating to obtain the aromatization catalyst. The use method is as follows: transforming oxy-compound raw materials to aromatic hydrocarbon through the catalyst under the reaction conditions. The nano ZSM-5 molecular sieve based catalyst has the characteristics of being high in aromatics yield (reaching up to 99%) and long in service life (the catalyst is alive after 300 hours, and the aromatics selectivity reaches up to 70% after the catalyst is subjected to hydrothermal aging at 760 DEG C for 4 hours).

Description

technical field [0001] The invention belongs to the technical field of preparation of aromatic hydrocarbons, and in particular relates to a nanometer ZSM-5 molecular sieve catalyst and its preparation and use methods. Background technique [0002] Aromatics such as benzene, toluene, p-xylene, trimethylbenzene, and tetramethylbenzene are important chemical raw materials, and their consumption is second only to ethylene and propylene. Among them, trimethylbenzene can prepare various dye intermediates such as trimellitic acid and benzoic anhydride, and can also be used to produce antioxidants, polyester resin curing agents, stabilizers, alkyd resin plasticizers, etc. Mesitylene is a good It is used as a developer for silicone photosensitive sheets in the electronics industry. Pyromellitic dianhydride obtained by oxidation of durene and diamine compounds can be polymerized to produce polyimide engineering plastics. At the same time, p-xylene (PX) can be produced by the disprop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J35/10B01J29/40C01B39/40C07C15/00C07C15/04C07C15/06C07C15/08C07C1/20
CPCY02P20/52
Inventor 魏飞马云海骞伟中
Owner TSINGHUA UNIV
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