A kind of method for preparing mesitylene from methanol and xylene

A technology of durene and xylene, which is applied in the field of durene preparation, can solve the problems of high cost, high reaction temperature and reaction pressure, and achieve the effects of high stability, reduced by-products and high activity

Active Publication Date: 2022-08-09
大连龙缘化学有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] But reaction temperature and reaction pressure are higher in the above-mentioned method, and cost is high

Method used

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  • A kind of method for preparing mesitylene from methanol and xylene

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Experimental program
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Effect test

Embodiment 1

[0038] Example 1 Preparation of modified nano-ZSM-5 molecular sieve catalyst

[0039] Mix the reaction raw materials 0.28g sodium metaaluminate, 0.44g sodium hydroxide and 21g deionized water uniformly, add 10g silica sol and mix well, add 1.2g n-butylamine and mix well, and then add 0.08g ZSM-5 seed crystal and mix well to form The mixed solution was added to the stirring tank, the stirring speed was adjusted to 300 r / min, the temperature was raised to 170 ° C for crystallization for 72 h, and the ZSM-5 molecular sieve carrier was obtained. The crystal grain size of the ZSM-5 molecular sieve carrier was about 220 nm. ZSM-5 molecular sieve carrier was impregnated with 0.5% sodium hydroxide solution at 80°C for 2 hours, then exchanged with 0.4M ammonium nitrate solution for 2 hours, and extruded into strips. The extruded ZSM-5 was treated with 0.2M hydrofluoric acid solution at 40°C for 4h, impregnated with 0.05% zinc nitrate for 24h, and calcined at 550°C for 6h to obtain the ...

Embodiment 2

[0040] Example 2 Preparation of modified nano ZSM-5 molecular sieve catalyst

[0041]Mix the reaction raw materials 0.31g sodium metaaluminate, 0.51g sodium hydroxide and 27g deionized water uniformly, add 10g silica sol and mix well, add 1.48g n-butylamine and mix well, then add 0.06g ZSM-5 seed crystal and mix well, A mixed solution is formed, the mixed solution is placed in a stirring tank, the stirring rate is adjusted to 300 r / min, the temperature is raised to 160 ° C for crystallization for 72 h, and a ZSM-5 molecular sieve carrier is obtained. The crystal grain size of the ZSM-5 molecular sieve carrier is about 300 nm. 5 g of the obtained ZSM-5 molecular sieve was treated with 0.4% sodium hydroxide solution at 80°C for 2 hours, then exchanged with 0.5M ammonium nitrate solution for 2 hours, and extruded into strips. The extruded ZSM-5 was treated with 0.2M sulfuric acid solution at 50°C for 4h, impregnated with 0.04% copper nitrate for 24h, and calcined at 550°C for 6h ...

Embodiment 3

[0043] Mix the reaction raw materials 0.34g aluminum isopropoxide, 0.41g sodium hydroxide and 25g deionized water, add 10g silica sol and mix well, add 0.87g n-butylamine and mix well, then add 0.09g ZSM-5 seed crystal and mix well, To form a mixed solution, add the mixed solution to the stirring tank, adjust the stirring speed to 300 r / min, and heat up to 170 ° C for crystallization for 72 h to obtain ZSM-5 molecular sieve. ZSM-5 molecular sieve was treated with 0.5% potassium hydroxide solution at 80°C for 2 hours, then exchanged with 0.6M ammonium nitrate solution for 1 hour, and extruded into strips. The extruded ZSM-5 was treated with 0.2M nitric acid solution at 30°C for 4h, impregnated with 0.05% magnesium nitrate for 24h, and calcined at 550°C for 6h to obtain a modified nano-ZSM-5 molecular sieve catalyst.

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Abstract

The invention provides a method for preparing mesitylene from methanol and xylene. The xylene is mixed with part of the methanol, and enters the reactor from the main line at the top, and the rest of the methanol enters the reactor through the multi-stage feeding method of the side line. , under the pressure of 0.5-2.0MPa, it is converted into mixed hydrocarbon components rich in mesitylene, and the heavy aromatic hydrocarbons rich in mesitylene are obtained after separation, and then through multi-stage freezing crystallization, centrifugal separation and pressing system to obtain high-purity homogenous hydrocarbons. Tetratoluene. The method adopts the multi-stage feed of side-line methanol to control the temperature rise of the bed during the alkylation, and makes full use of the reaction heat of the upper bed of the reactor to keep the middle and end beds warm, and uses a modified nano-ZSM-5 molecular sieve catalyst to obtain heat preservation. The reaction temperature is lowered; the alkylation of xylene and its mixed aromatics with methanol continuously improves the selectivity of mesitylene in the oil phase product. Moreover, the yield of mesitylene is improved by making full use of the reaction by-products.

Description

technical field [0001] The invention relates to a preparation method of mesitylene in the technical field of aromatic hydrocarbon production chemical industry, in particular to a method for preparing mesitylene from methanol and xylene. Background technique [0002] 1,2,4,5-Tetramethylbenzene (1,2,4,5-tetramethylbenzene), commonly known as durene, is an important organic chemical raw material, mainly used for the production of pyromellitic dianhydride and then polyimide. With the continuous expansion of the market amount of polyimide, the demand for mesitylene as the main raw material for the synthesis of polyimide is also increasing day by day. [0003] At present, the synthesis process of mesitylene includes methanol alkylation of mesitylene; isomerization and disproportionation of mesitylene; chloromethylation of mesitylene; isomerization of tetratoluene; methanol to mesitylene, etc. The demand for mesitylene is increasing day by day, so it is urgent to explore new raw m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/86C07C15/02B01J29/40B01J29/46B01J37/30B01J37/06B01J37/02B01J37/08B82Y30/00B82Y40/00
CPCC07C2/864B01J29/40B01J29/405B01J29/46B01J37/30B01J37/06B01J37/0201B01J37/082B82Y30/00B82Y40/00C07C15/02Y02P20/52
Inventor 王刃王相珣张伶超徐连海吴昊袁麟
Owner 大连龙缘化学有限公司
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