Modified ZSM-5 molecular sieve catalyst, preparation method and application in toluene methanol alkylation reaction

A technology of ZSM-5 and molecular sieve, which is applied in molecular sieve catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of not being able to use aromatic hydrocarbon raw materials, and achieve high selectivity, high activity selectivity, and high activity Effect

Inactive Publication Date: 2012-10-10
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mobil's TDP and the subsequent STDP technology are mainly based on ZSM-5 molecular sieve catalysts, wh...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 6 grams of ZSM-5 molecular sieve raw powder (Nankai University molecular sieve factory, the same below), add TEOS dissolved in cyclohexane (100ml), the concentration is 0.0044mol / mL, and react continuously at 60°C for 5h. After the reaction was completed, centrifuged, the sample was dried and calcined in an air atmosphere at 550°C for 3 hours to obtain SiO 2 Deposit modified ZSM-5 molecular sieve samples. After XRF analysis, its SiO 2 The deposition amount is about 2.9%.

[0018] Get above-mentioned catalyst 0.5g, carry out toluene methanol alkylation continuous reaction in fixed-bed reactor, reaction temperature is 470 ℃, reaction pressure is normal pressure, reaction atmosphere is nitrogen, reaction material is toluene-methanol mixture (molar ratio 2: 1), liquid space velocity 2h -1 , Carrier gas / liquid material molar ratio = 5:1. After 2 hours, sampling and chromatographic analysis showed that the conversion rate of toluene was 43.2%, the selectivity (p-X) of...

Embodiment 2

[0020] Take 10g of conventional particle size ZSM-5 molecular sieve powder, put it in a thin layer in an evaporating dish, put it in a constant temperature and humidity control box, control the dry bulb temperature to 70°C, wet bulb temperature to 71°C, and relative humidity to 83%. Humidification treatment for 1 hour. Take 6 grams of ZSM-5 molecular sieve after humidification treatment, add TEOS dissolved in cyclohexane (100ml), the concentration is 0.1844mol / mL, and react continuously at 60°C for 5h. After the reaction was completed, centrifuged, the sample was dried and calcined in an air atmosphere at 550°C for 3 hours to obtain SiO 2 Deposit modified molecular sieve samples. After XRF analysis, its SiO 2 The deposition amount is about 25.0%.

[0021] Get above-mentioned catalyst 0.5g, carry out toluene methanol alkylation continuous reaction in fixed-bed reactor, reaction temperature is 470 ℃, reaction pressure is normal pressure, reaction atmosphere is nitrogen, react...

Embodiment 3

[0023] Take 10g of small particle size ZSM-5 molecular sieve raw powder, place it in a thin layer on an evaporating dish, put it in a constant temperature and humidity control box, control the dry bulb temperature at 65°C, wet bulb temperature at 60°C, and relative humidity at 78%. Humidification treatment for 1 hour. Take 6 grams of ZSM-5 molecular sieve sample after humidification treatment, add TEOS dissolved in cyclohexane (100ml), the concentration is 0.0407mol / mL, and react continuously at 60°C for 5h. After the reaction was completed, centrifuged, the sample was dried and calcined in an air atmosphere at 550°C for 3 hours to obtain SiO 2 Deposit modified molecular sieve samples. After XRF analysis, its SiO 2 The deposition amount is about 17.0%, and the SiO 2 Deposit modified small particle size ZSM-5 molecular sieve samples.

[0024] Get above-mentioned catalyst 0.5g, carry out toluene methanol alkylation continuous reaction in fixed-bed reactor, reaction temperatu...

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Abstract

The invention relates to a modified ZSM-5 molecular sieve catalyst used for toluene methanol alkylation, which takes a ZSM-5 molecular sieve as a matrix, molecular sieve raw powder is taken as a commodity reagent, its scaled silica-alumina ratio (nSiO2/nAl2O3) is 25, the particle sizes can be divided into two types, the primary particle size of the large particle size (or conventional particle size) ZSM-5 belongs to the micron order, the primary particle size of the small particle size ZSM-5 is about 200 nanometers, tetraethoxysilane (TEOS) is taken as a silicon source, an external surface and hole opening of the molecular sieve can be modified through chemical liquid phase deposition, the SiO2 deposition amount is between 3% and 25%, or chemical modification of Ni and P elements is employed, and the contents of Ni and P elements are 0-1% and 0-8%. According to the invention, the modified ZSM-5 molecular sieve catalyst can be used for preparing xylene by the toluene methanol alkylation with high catalytic activity, the conversion for per pass of toluene can reach more than 30%, in three types of xylene products, the selectivity on xylene is higher than 90%, and the modified ZSM-5 molecular sieve catalyst of the invention is the catalyst possessing high activity and high selectivity.

Description

technical field [0001] The present invention relates to ZSM-5 molecular sieve catalyst and toluene methanol alkylation. Background technique [0002] Through toluene disproportionation and transalkylation, benzene and xylene can be generated from toluene and from toluene and C 9 Aromatics generate xylene, and the process is characterized by not generating ethylbenzene. At present, the processes that have been industrialized abroad mainly include Xylene-Plus of ARCO Company, Tatoray Technology of Toray Company, Toluene Disproportionation (TDP) and Selective Toluene Disproportionation (STDP) technology of Mobil Company, and UOP Company's PX-Plus technology. Among them, xylene production stimulation technology was developed earlier, using moving bed reactor, non-hydrogen operation, low operating cost, but the catalyst is easy to coke and deactivate; mixed xylenes have more meta-products, but the selectivity of para-products is not high . Tatoray technology adopts adiabatic ...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J29/46C07C15/06C07C15/08C07C2/88
CPCY02P20/52
Inventor 季伟捷陆平费兆阳赵亮丁维平陈懿杨为民谢在库
Owner NANJING UNIV
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