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Method for preparing 2, 6-dimethylphenol

A technology of dimethylphenol and o-cresol, which is applied in two fields, can solve the problems of short life of ortho-methylation catalysts and lower production efficiency, and achieve the goals of shortening product production cycle, improving production efficiency and reducing production cost Effect

Inactive Publication Date: 2005-07-06
芮城福斯特化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Just because the life-span of existing ortho-position methylation catalyst is relatively short, make in the synthetic of 2,6-xylenol need to change catalyst frequently, have reduced the production efficiency of continuous production, meanwhile, due to ortho-position methylation However, some of the above-mentioned problems still exist in the catalyst, which also makes the phenol conversion rate and ortho-position selectivity in the synthesis of 2,6-dimethylphenol have room for further optimization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Preparation of catalyst

[0046] Weigh 50KgFe(NO 3 ) 3 9H 2 O, 3KgInCl 3 4H 2 O, 500gCr(NO 3 ) 3 9H 2 O, 300gNa 2 SiO 3 9H 2 O and 60gCaCl 2 2H 2 O, dissolved in 1000L of water, first dropwise add 10% ammonia water to neutralize the solution to pH = 7.0, then continue to neutralize with 10% ammonia water to pH = 7.5-8.0, stir for 1 hour, and leave the solution to age for 12 hours. The deposited precipitate was filtered, washed with water, and dried at 180°C for 6 hours. The dried sediment is crushed into 8-10 mesh particles, put into 20L of 0.5% K 2 CO 3 After immersing in the solution for 16 hours at room temperature, filter and separate, dry the obtained particles at 150°C for 6 hours, and then bake them in a roasting furnace at 480°C for 5 hours. Finally, add 100g of graphite to the calcined product, mix well and then press it into a cylinder of Φ3×3mm to obtain a composite of iron oxide, indium oxide, silicon dioxide, chromium oxide, calcium oxide,...

Embodiment 2

[0051] 1. Preparation of catalyst

[0052] Weigh 55KgFe(NO 3 ) 3 9H 2 O, 3.5KgInCl 3 4H 2 O, 500gCrCl 3 ·6H 2 O, 730gNa 2 SiO 3 9H 2 O and 75gCaCl 2 2H 2 O, dissolved in 1000L of water, heated to 90°C, neutralized to pH=7.5-8.0 by adding urea, stirred for 1 hour, and left to age the solution for 12 hours. The deposited precipitate was filtered, washed with water, and dried at 150°C for 5 hours. The dried sediment is crushed into 8-10 mesh particles, put into 30L of 1% Cs 2 CO 3 with 0.5% K 2 CO 3 After immersing in the mixed solution at room temperature for 18 hours, filter and separate, dry the obtained particles at 150°C for 4 hours, and then bake them in a roasting furnace at 400°C for 8 hours. Finally, add 50g of graphite to the calcined product, mix well and then press it into a cylinder of Φ3×3mm to obtain a composite of iron oxide, indium oxide, silicon dioxide, chromium oxide, calcium oxide, cesium oxide, oxide A catalyst composed of potassium and grap...

Embodiment 3

[0057] 1. Preparation of catalyst

[0058] Weigh 42.4KgFeCl 3 ·6H 2 O, 250gCrCl 3 ·6H 2 O, 550gNa 2 SiO 3 9H 2 O and 100g CaCl 2 2H 2 O, dissolved in 800L of water, weighed 1.5Kg elemental indium and dissolved in 0.8L of hydrochloric acid, after all dissolved, added to the above solution, first dropwise added 10% ammonia water to neutralize the solution to pH = 7.0, and then continue Neutralize to pH=7.5-8.0 with 10% ammonia water, stir for 1 hour, and leave the solution to age for 12 hours. The deposited precipitate was filtered, washed with water, and dried at 180°C for 6 hours. The dried sediment is crushed into 8-10 mesh particles, put into 20L of 1.27% Cs 2 CO 3 After immersing in the solution for 18 hours at room temperature, filter and separate, dry the obtained particles at 180°C for 3 hours, and then bake at 480°C for 5 hours in a roasting furnace. Finally, add 30g of graphite to the calcined product, mix well and then press it into a cylinder of Φ3×3mm to...

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PUM

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Abstract

The preparation method of 2,6-dimethylphenol is to pass the reaction material mixed with methanol and water at a liquid space velocity of 0.5-2.0h-1 through a The fixed-bed reactor of the ortho-methylation catalyst is used for gas-phase catalytic reaction at 280-400°C and 0-1.5Mpa pressure to prepare 2,6-dimethylphenol. The ortho-methylation catalyst is composed of iron oxide, indium oxide, silicon dioxide, oxide Chromium, calcium oxide, alkali metal oxides and graphite. The phenol conversion rate of synthesizing 2,6-xylenol in the invention reaches 99 percent, the ortho position selectivity reaches 97 percent, and the service life of the catalyst reaches more than 3000 hours.

Description

Technical field [0001] The present invention relates to a kind of preparation method of 2,6-xylenol, more specifically, relate to a kind of phenolic compound and methanol to carry out gas phase catalysis under the action of ortho-position methylation catalyst, to prepare 2,6- Dimethylphenol method. Background technique [0002] 2,6-Dimethylphenol is an important monomer and engineering plastic modifier for the synthesis of polyphenylene ether heat-resistant resin (PPE), and is also an important synthetic raw material for some pharmaceutical intermediates, and is widely used. [0003] Early 2,6-dimethylphenol was isolated from coal tar and petroleum cracking products, with low yield and poor quality. In 1945, N. Cullinane and others first used phenol and methanol for gas-phase catalytic methylation to synthesize 2,6-dimethylphenol. Subsequently, engineers from various countries have repeatedly improved the preparation method, which mainly involves the improvement of the cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/11C07C39/07
Inventor 张小林刘永红赵建朝
Owner 芮城福斯特化工有限公司
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