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Method for preparing durene from methanol and xylene

A technology of mesitylene and xylene, applied in the field of preparation of mesitylene, can solve the problems of high reaction temperature and reaction pressure, high cost, and achieve the effects of reducing by-products, high stability and lowering reaction temperature

Active Publication Date: 2019-12-31
大连龙缘化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Method for preparing durene from methanol and xylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1 Preparation of modified nanometer ZSM-5 molecular sieve catalyst

[0039] Mix the reaction raw materials 0.28g sodium metaaluminate, 0.44g sodium hydroxide and 21g deionized water evenly, add 10g silica sol and mix evenly, add 1.2g n-butylamine and mix evenly, then add 0.08g ZSM-5 seed crystals and mix evenly to form Mixed solution, put the mixed solution into a stirring tank, adjust the stirring rate to 300r / min, raise the temperature to 170°C to crystallize for 72 hours, and obtain a ZSM-5 molecular sieve carrier. The grain size of the ZSM-5 molecular sieve carrier is about 220nm, and 5g is obtained. The ZSM-5 molecular sieve carrier was impregnated with 0.5% sodium hydroxide solution at 80° C. for 2 hours, then exchanged with 0.4 M ammonium nitrate solution for 2 hours, and extruded. 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 m...

Embodiment 2

[0040] Embodiment 2 Preparation of modified nanometer ZSM-5 molecular sieve catalyst

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

Embodiment 3

[0043] Mix the reaction raw materials 0.34g aluminum isopropoxide, 0.41g sodium hydroxide and 25g deionized water evenly, add 10g silica sol and mix evenly, add 0.87g n-butylamine and mix evenly, then add 0.09g ZSM-5 seed crystal and mix evenly, Form a mixed solution, put the mixed solution into a stirring tank, adjust the stirring rate to 300r / min, raise the temperature to 170°C to crystallize for 72 hours, and obtain a ZSM-5 molecular sieve. The grain size of the ZSM-5 molecular sieve carrier is about 210nm, and 5g is obtained. ZSM-5 molecular sieves were 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. 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 the modified nano ZSM-5 molecular sieve catalyst.

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Abstract

The invention provides a method for preparing durene from methanol and xylene. Xylene is mixed with a part of methanol; the mixture enters from a top main line into a reactor, and the rest methanol enters the reactor in a side-line multi-section feeding manner; the materials are converted into a mixed hydrocarbon component rich in durene under the conditions that the temperature is 250-400 DEG C and the pressure intensity is 0.5-2.0 MPa, the mixed hydrocarbon component is separated to obtain heavy aromatic hydrocarbon rich in durene, and through multi-stage freezing crystallization and centrifugal separation squeezing system, high-purity durene is obtained. Bed layer temperature rise during alkylation is controlled by adopting side line methanol multi-section feeding, reaction heat of an upper-section bed layer of the reactor is fully utilized to preserve heat of a middle-section bed layer and a tail-section bed layer, and a modified nano ZSM-5 molecular sieve catalyst is used for reducing the reaction temperature; xylene and mixed aromatic hydrocarbon thereof and methanol are continuously subjected to alkylation reaction for many times, so that the selectivity of durene in an oilphase product is improved. And the yield of durene is improved by fully utilizing reaction by-products.

Description

technical field [0001] The invention relates to a method for preparing durene in the technical field of aromatics production and chemical engineering, in particular to a method for preparing durene with methanol and xylene. Background technique [0002] Durene (1,2,4,5-tetramethylbenzene), commonly known as durene, is an important organic chemical raw material, mainly used to produce pyromellitic dianhydride, and then to produce polyimide. As the market usage of polyimide continues to expand, the demand for durene as the main raw material for synthesizing polyimide is also increasing day by day. [0003] The current synthetic method of durene includes alkylation of mesitylene with methanol; isomerization and disproportionation of mesitylene; chloromethylation of mesitylene; isomerization of mesitylene; production of mesitylene from methanol, etc. The demand for durene is increasing day by day, so it is imminent to explore new raw materials and process routes for preparing d...

Claims

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Application Information

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Patent Type & Authority Applications(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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