Phenol ortho-methylation catalyst and preparation method thereof

A catalyst and methylation technology, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of unfavorable environmental protection, high reaction temperature, and low selectivity of o-cresol, etc. High stability, low reaction temperature, good stability

Active Publication Date: 2009-08-26
HUNAN XINLING CHEM CO LTD
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  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new type of catalyzer can be used with different chemicals without causing harm or discomfort during use. It'll have excellent performance at lower temperatures than current methods like methanols due to its stable structure.

Problems solved by technology

This patented technical problem addressed in the patents relating to the use of different types of catalysis system with specific advantages or disadvantages depending upon their desired outcome.

Method used

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  • Phenol ortho-methylation catalyst and preparation method thereof
  • Phenol ortho-methylation catalyst and preparation method thereof

Examples

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Effect test

Embodiment 1

[0020] Weigh Fe(NO 3 ) 3 9H 2 O 404g and Mg(NO 3 ) 2 ·6H 2 O 51.2g was mixed and dissolved in 800mL ethanol, and then it was slowly mixed with 700mL of 28% concentrated ammonia water containing 4g PEG in parallel flow under ultrasonic conditions at room temperature. Wash and dry at 120°C for 6h. The obtained solid is calcined at 450°C for 8 hours, and finally the solid is ground into fine particles, and then crushed into small particles of 10-20 meshes, which is the obtained catalyst Fe. 1 Mg 0.2 / o.

[0021] The above-mentioned catalyst is packed in a stainless steel tube with an inner diameter of Φ7mm, the packing mass is 8g, the reaction temperature is 310°C, the raw material is phenol:methanol:water=1:4:3 (both are molar ratios), and the feed space velocity is 1.0 h -1 , the carrier gas is N 2 The flow rate was 25mL / min, the reaction was 24h, the conversion rate of phenol was 47.3%, the selectivity of o-cresol was 90.2%, and the selectivity of 2,6-xylenol was 9.7...

Embodiment 2

[0023] Weigh anhydrous Fe(OAc) 3 233g and Mg(OAc) 2 Mix and dissolve 284g in 800mL ethanol, then slowly mix it with 1000mL of 28% concentrated ammonia water containing 8g PEG in parallel flow under the condition of ultrasonic at room temperature, continue to ultrasonicate for 30min after adding, then filter the precipitate, wash, Bake at 120°C for 6h. The obtained solid is calcined at 450°C for 8 hours, and finally the solid is ground into fine particles, and after being pressed into tablets, it is crushed into small particles of 10-20 meshes, which is the catalyst Fe obtained. 1 Mg 2 / o.

[0024] The prepared catalyst was filled in a stainless steel tube with an inner diameter of Φ7mm, the filling mass was 8g, the reaction temperature was 350°C, the raw material was phenol:methanol:water=1:4:3 (both in molar ratio), and the feed space velocity was 1.0h -1 , the carrier gas is N 2 The flow rate was 25mL / min, the reaction was 24h, the conversion rate of phenol was 48.6%, ...

Embodiment 3

[0026] Weigh Fe(NO 3 ) 3 9H 2 O 404g, Mg(NO 3 ) 2 ·6H 2 O 25.6g and Ce(NO 3 ) 3 ·6H 2 O2.17g was mixed and dissolved in 800mL ethanol, and then it was slowly mixed with 28% 700mL concentrated ammonia water containing 0.8g PEG in a parallel flow under ultrasonic conditions at room temperature. , washed, and baked at 120°C for 6h. The obtained solid is calcined at 450°C for 8 hours, and finally the solid is ground into fine particles, and then crushed into small particles of 10-20 meshes, which is the obtained catalyst Fe. 1 Mg 0.1 Ce 0.01 / o.

[0027] The catalyst loading method and reaction conditions are the same as in Example 1, and the reaction results are shown in Table 1.

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Abstract

The invention discloses a phenol ortho-methylation catalyst and a preparation method thereof. The catalyst is an alkaline Fe/Mg compound oxide, wherein, the mol ratio of Fe to Mg is 1: (0.1-2). The preparation method comprises the following steps: mixing and dissolving soluble malysite and soluble magnesium salts into alcohols solvent according to a required proportion to prepare a solution A; adding polyethyleneglycol (PEG) into strong aqua ammonia to prepare a solution B; slowly mixing the solution A and the solution B in a cocurrent flow mode under the condition of normal temperature and ultrasound, and then going on with the ultrasound for 30 minutes; filtering, washing, drying and baking the obtained precipitation; porphyrizing the baked solid and repulverizing the solid into 10-20 mesh finely ground particles after tabletting; the finely ground particles are the catalyst. The catalyst has the advantages of high activity at low temperature, simple preparation, innocuity, good stability, high selectivity of ortho position, particularly high selectivity of orthocresol and few by-products.

Description

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Claims

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Application Information

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Owner HUNAN XINLING CHEM CO LTD
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