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Method for preparing o-cresol

A technology for o-cresol and phenol, applied in the field of preparing o-cresol, can solve the problem of low selectivity of o-cresol, and achieve the effects of long service life, low selectivity and high selectivity

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

AI Technical Summary

Problems solved by technology

[0007] In all existing industrial synthesis methods of ortho-cresol, the selectivity of ortho-cresol is not high, and more by-products such as 2,6-xylenol, m-cresol, p-cresol, benzene, etc. are usually generated. Ether and other advanced alkylation products, among which 2,6-xylenol is the main by-product

Method used

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  • Method for preparing o-cresol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Catalyst preparation: Weigh Fe(NO 3 ) 3 9H 2 O 404g, Mg(NO 3 ) 2 ·6H 2 O 51.2g and Ce(NO 3 ) 3 ·6H 2 O 2.17g was mixed and dissolved in 800mL ethanol, and then it was slowly mixed with 28% concentrated ammonia water 700mL containing 4g PEG in a co-current manner under normal temperature ultrasonic conditions, and the ultrasonic wave was continued for 30min after the addition, and then the precipitate was filtered. Wash and dry at 120°C for 6h. The obtained solid is then roasted at 450°C for 8 hours, and finally the solid is ground into fine particles, and then crushed into small particles of 10 to 20 meshes after tableting. The obtained basic metal oxide catalyst is Fe 1 Mg 0.2 Ce 0.05 / o.

[0027] The above-mentioned catalyst was packed in a Φ7mm stainless steel reaction tube, the catalyst loading amount was 5g, the reaction mixture was metered in with an advection pump, and the temperature was controlled by a temperature control device. Feed space velocity...

Embodiment 2

[0032] Catalyst is with embodiment 1. Reaction mixture phenol / methanol / water=1 / 4 / 3 (mol / mol), carrier gas helium flow rate is 30mL / min, changes reaction temperature, other conditions are with embodiment 1, reacted 12 hours sampling and carried out chromatographic analysis, o-formazan The phenol selectivity is above 89.5%, and the ortho position selectivity is above 99.1%. The results are shown in Table 2.

[0033] Table 2 changes the result of reaction temperature synthesis o-cresol

[0034]

Embodiment 3

[0036] Catalyst is with embodiment 1. Reaction mixture phenol / methanol / water=1 / 4 / 3 (mol / mol), change feeding space velocity, other conditions are with embodiment 1, react 12 hours sampling and carry out chromatographic analysis, o-cresol selectivity is more than 89.7%, o-cresol The position selectivity is above 99.2%, and the results are shown in Table 3.

[0037] Table 3 changes the result of feed space velocity synthesis o-cresol

[0038]

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Abstract

The invention discloses a method for preparing o-cresol, which is characterized by comprising the following steps: uniformly mixing phenol with methanol by a mass ratio 1: (0.5-4), and then pumping the mixture into a reaction tube containing alkylate catalyst, introducing inert carrier gas into the reaction tube, and obtaining o-cresol after condensing and recycling the reaction product. The reaction conditions comprise normal atmosphere, reaction temperature of 280 to 450 DEG C, and the airspeed of incoming stock of 0.8-1.8h. The method has advantages of simple technical process, high selectivity of o-cresol, no generation of by-products such as meta-cresol, p-cresol and anisole relatively low selectivity of 2, 6-dimethyl phenol and long service life of the catalyst.

Description

technical field [0001] The invention relates to a method for preparing o-cresol, in particular to a method for preparing o-cresol with basic metal oxides as catalysts and phenol and methanol as raw materials. Background technique [0002] o-cresol, also known as o-cresol, is a colorless crystal with a strong phenol smell, slightly soluble in water, soluble in ethanol, ether, chloroform and hot water, and is mainly used as a synthetic resin, pesticide, medicine, dye, and antioxidant and other raw materials. [0003] The methods for industrial production of o-cresol include: natural separation method, o-toluidine diazotization method, toluene chlorination hydrolysis method, and phenol-methanol alkylation method. The first three methods have complex process, serious environmental pollution, and many by-products, and are generally not used in large-scale industrial production at present. [0004] The phenol-methanol alkylation method uses phenol and methanol as raw materials t...

Claims

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Application Information

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IPC IPC(8): C07C39/07C07C37/16B01J23/78
Inventor 黄华衷晟佘喜春徐斌谢琼玉胡莲佑
Owner HUNAN XINLING CHEM CO LTD
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