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Preparation method of micron-sized HZSM-5 molecular sieve and application of micron-sized HZSM-5 molecular sieve

A molecular sieve, micron-scale technology, applied in molecular sieve catalysts, chemical instruments and methods, hydrocarbon production from halogen-containing organic compounds, etc., can solve the problems such as the inconspicuous advantage of xylene diffusion, achieve simple and easy preparation process, and improve para-position Selectivity, catalytic activity and selective effect

Inactive Publication Date: 2017-05-10
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the relatively short diffusion channel, the diffusion advantage of p-xylene is not obvious

Method used

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  • Preparation method of micron-sized HZSM-5 molecular sieve and application of micron-sized HZSM-5 molecular sieve
  • Preparation method of micron-sized HZSM-5 molecular sieve and application of micron-sized HZSM-5 molecular sieve
  • Preparation method of micron-sized HZSM-5 molecular sieve and application of micron-sized HZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] According to the molar ratio of material SiO 2 :Al 2 o 3 :TPAOH:TEA:NaOH:H 2 The ratio of O=100:0.67:30:10:16.5:3800, with 20.03g silica sol (30wt.%), 0.446g aluminum sulfate, 24.402g tetrapropyl ammonium hydroxide (25wt.%), 1.012g triethyl Amine, 0.660g sodium hydroxide and water, mix well, statically crystallize at 180°C for 24h, cool, centrifuge, wash with water until neutral, dry overnight, then place in a muffle furnace and gradually raise the temperature to 550°C, and roast for 5h to obtain Molecular sieve Na-ZSM-5; ion exchange with 1mol / L ammonium nitrate solution at 80°C for 3h, repeat once, wash with water, dry overnight, put in a muffle furnace and gradually raise the temperature to 550°C, and roast for 5h to obtain Si / Al =75 HZSM-5 molecular sieve A.

[0029] Molecular sieve catalyzed methyl bromide toluene to prepare p-xylene reaction is carried out in a miniature fixed bed quartz reactor, take 1g of the above catalyst, nitrogen carrier gas flow rate 10...

Embodiment 2

[0031] According to the molar ratio of material SiO 2 :Al 2 o 3 :TPAOH:TEA:NaOH:H 2 The ratio of O=100:0.67:20:20:16.5:3800, with 20.03g silica sol (30wt.%), 0.446g aluminum sulfate, 16.268g tetrapropyl ammonium hydroxide (25wt.%), 2.024g triethyl Amine, 0.660g sodium hydroxide and water, mix well, statically crystallize at 180°C for 24h, cool, centrifuge, wash with water until neutral, dry overnight, then place in a muffle furnace and gradually raise the temperature to 550°C, and roast for 5h to obtain Molecular sieve Na-ZSM-5; ion exchange with 1mol / L ammonium nitrate solution at 80°C for 3h, repeat once, wash with water, dry overnight, put in a muffle furnace and gradually raise the temperature to 550°C, and roast for 5h to obtain Si / Al =75 HZSM-5 Molecular Sieve B.

[0032] Molecular sieve catalyzed methyl bromide toluene to prepare p-xylene reaction is carried out in a miniature fixed bed quartz reactor, take 1g of the above catalyst, nitrogen carrier gas flow rate 10...

Embodiment 3

[0034] According to the molar ratio of material SiO 2 :Al 2 o 3 :TPAOH:TEA:NaOH:H 2 The ratio of O=100:0.67:10:30:16.5:3800, with 20.03g silica sol (30wt.%), 0.446g aluminum sulfate, 8.134g tetrapropyl ammonium hydroxide (25wt.%), 3.036g triethyl Amine, 0.660g sodium hydroxide and water, mix well, statically crystallize at 180°C for 24h, cool, centrifuge, wash with water until neutral, dry overnight, then place in a muffle furnace and gradually raise the temperature to 550°C, and roast for 5h to obtain Molecular sieve Na-ZSM-5; ion exchange with 1mol / L ammonium nitrate solution at 80°C for 3h, repeat once, wash with water, dry overnight, put in a muffle furnace and gradually raise the temperature to 550°C, and roast for 5h to obtain Si / Al =75 HZSM-5 molecular sieve C.

[0035] Molecular sieve catalyzed methyl bromide toluene to prepare p-xylene reaction is carried out in a miniature fixed bed quartz reactor, take 1g of the above catalyst, nitrogen carrier gas flow rate 10m...

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Abstract

The invention discloses a micron-sized HZSM-5 molecular sieve catalyst. According to the micron-sized HZSM-5 molecular sieve catalyst disclosed by the invention, the micron-sized HZSM-5 molecular sieve is designed and synthesized by utilizing double-template, and thus, not only can acidity of the surface of a zeolite catalyst be modulated but also a diffusion path of a product can grow by increasing a particle size, and then, the goal of increasing para-selectivity is achieved. The invention further provides a preparation method of the micron-sized HZSM-5 molecular sieve and catalytic application of the micron-sized HZSM-5 molecular sieve. The micron-sized HZSM-5 molecular sieve catalyst provided by the invention is synthesized by a double-template one-step hydrothermal method, so that the preparation process is simple and convenient; when being applied to methyl bromide methylated methylbenzene to prepare paraxylene, the molecular sieve shows higher catalytic activity and selectivity during reaction; the catalyst shows the higher selectivity, which dues to fewer strong acid sites and a larger grain size; moreover, the catalyst has no corrosion on a fixed bed reactor, and generated hydrogen bromide tail gas is easy to recycle, so that the catalyst belongs to an environmentally friendly catalyst; and after being deactivated, the catalyst can be repeatedly used for more than once through simple roasting.

Description

[0001] 【Technical field】 [0002] The invention relates to the technical field of preparation and application of zeolite catalytic materials, in particular to a preparation method and application of a micron-sized HZSM-5 molecular sieve. [0003] 【Background technique】 [0004] Paraxylene (PX) is an important basic chemical raw material, which is widely used in many chemical production fields such as polyester fiber, plastic, pesticide, medicine, etc., especially as a raw material for synthetic polyester fiber and plastic , the demand for p-xylene is also increasing. At present, p-xylene is mainly obtained by selective disproportionation of toluene, adsorption separation or crystallization separation of mixed xylenes. However, the production cost of these processes is relatively high; in addition, in the selective disproportionation process of toluene, a large amount of by-product benzene is generated. In recent years, the preparation of p-xylene by alkylating toluene with me...

Claims

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Application Information

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IPC IPC(8): C01B39/40B01J29/40C07C1/26C07C15/08
CPCY02P20/52Y02P20/584C01B39/40B01J29/40C01P2004/61C07C1/26C07C15/08
Inventor 尹双凤谢军陈浪王无悔王朋
Owner HUNAN UNIV
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