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Method of producing methylphenol by gas-phase alkylation of phenol and methanol

A technology of alkylation and methanol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as environmental pollution and equipment corrosion

Active Publication Date: 2014-02-12
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no industrial device for the production of cresol by molecular sieve-catalyzed gas-phase alkylation of phenol and methanol at home and abroad. The traditional industrial production route of cresol uses strong acid and strong alkali, and a large amount of industrial wastewater is generated during the production process. The environment is seriously polluted and the equipment is corroded.

Method used

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  • Method of producing methylphenol by gas-phase alkylation of phenol and methanol
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  • Method of producing methylphenol by gas-phase alkylation of phenol and methanol

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The preparation process of the catalyst is as follows: 120 grams of ZSM-5 molecular sieve with a molar silicon-aluminum ratio of 20 is mixed with 60 grams of diatomaceous earth, 100 grams of silicon dioxide weight 20% silica sol, and an appropriate amount of 10% dilute nitric acid is added as an extrusion aid Extrusion molding. Dry at 120°C and bake at 500°C for 10 hours. The above catalyst was cut into 1-3 mm to prepare columnar catalyst precursor A0. 20 grams of precursor catalyst A0 was added to 50 ml of nitric acid solution with a weight content of 10%, and soaked at room temperature for 4 hours. Dry at 120°C and bake at 550°C for 10 hours to prepare A1. Add 7.5 g of a cyclohexane solution of 50% by weight benzyl silicone oil to 20 g of A1, and soak at room temperature for 2 hours. Dry at 120°C, and then bake at 550°C for 2 hours to obtain A2. Immerse 20 grams of A2 sample with ammonium dihydrogen phosphate aqueous solution for 12 hours, dry at 120°C, and roast a...

Embodiment 2

[0031] The preparation process of the catalyst is as follows: 170 grams of ZSM-5 molecular sieve with a molar silicon-aluminum ratio of 30 is mixed with 100 grams of silicon dioxide and 30% silica sol by weight, and an appropriate amount of 10% dilute nitric acid is added as an extrusion aid to extrude. Dry at 120°C and bake at 700°C for 4 hours. The above catalyst was cut into 1-3mm to prepare columnar catalyst matrix B0. Add 50ml of ammonium nitrate solution with a weight content of 10% to 20 grams of matrix catalyst B0 and soak at room temperature for 10 hours. B1 was prepared by drying at 120°C and calcining at 600°C for 2 hours. Add 7.5 g of a cyclohexane solution of 50% by weight benzyl silicone oil to 20 g of B1, and soak at room temperature for 24 hours. Dry at 120°C, and then bake at 800°C for 2 hours to obtain B2. Immerse 20 grams of B2 sample in ammonium dihydrogen phosphate aqueous solution for 12 hours, dry at 120°C, and roast at 550°C for 10 hours, P 2 o 5 Th...

Embodiment 3

[0033] The preparation process of the catalyst is as follows: 200 grams of ZSM-5 molecular sieve with a molar silicon-aluminum ratio of 400 is mixed with 20 grams of diatomaceous earth, 100 grams of silicon dioxide weight 30% silica sol, and an appropriate amount of 10% dilute nitric acid is added as an extrusion aid Extrusion molding. Dry at 120°C and bake at 550°C for 4 hours. The above-mentioned catalyst was cut into 1-3 mm to prepare columnar catalyst matrix D0. 20 grams of matrix catalyst D0 was added to 50 ml of nitric acid solution with a weight content of 10%, and soaked at room temperature for 24 hours. D1 was obtained by drying at 120°C and calcining at 600°C for 3 hours. Add 7.5 g of a cyclohexane solution of 50% by weight benzyl silicone oil to 20 g of D1, and soak at room temperature for 24 hours. D21 was prepared by drying at 120°C and then calcining at 500°C for 3 hours. Add 7.5 g of a 50% by weight simethicone solution in n-hexane to 20 g of D21, and soak at...

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Abstract

The invention relates to a method of producing methylphenol by gas-phase alkylation of phenol and methanol. The phenol and the methanol after being preheated are mixed with a diluent gas, pass continuously through a catalyst bed layer of the phenol-methanol alkylation, and are subjected to a gas-phase reaction at a temperature of 200-500 DEG C and at a feed weight hourly space velocity of 0.5-20 h<-1> to produce the methylphenol. A phenol-methanol alkylation catalyst is prepared by modification using MCM-22, ZSM-5 and a beta molecular sieve as active components. The phenol and the methanol are used as raw materials. The methylphenol selectivity can reach 90%, and the para-position selectivity can reach 58%. The catalyst is good in stability. Producing processes are free from equipment corrosion. The catalyst is environmental friendly and has a good industrial application prospect.

Description

technical field [0001] The invention relates to a method for producing cresol, in particular to a method for producing cresol by vapor-phase alkylation of phenol and methanol. Background technique [0002] p-cresol is a colorless liquid or crystal with a special smell, corrosive and toxic, insoluble in water, easily soluble in alkaline solution or toluene, ethanol and other organic solvents, is an important fine chemical raw material, widely used in Antioxidants, dyes, pharmaceuticals, pesticides, spices and other industries. o-cresol, also known as: 2-cresol, o-cresol is an important fine chemical intermediate for the synthesis of pesticides, medicines, dyes, synthetic resins, spices, antioxidants, etc. m-cresol, also known as 3-cresol, m-cresol, and m-cresol, are mainly used as pesticide intermediates to produce insecticides such as fenitrothion, fenthion, medicarb, and permethrin. Intermediates for color films, resins, plasticizers and fragrances. Coal tar phenol conta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/07C07C37/16B01J29/40B01J29/03B01J29/70
CPCB01J29/40B01J29/7007B01J29/7038B01J2229/126B01J2229/26B01J2229/32B01J2229/36B01J2229/37C07C37/16C07C39/07
Inventor 王坤院徐云鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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