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A kind of method that takes molecular sieve as catalyst to produce cresol

A molecular sieve and catalyst technology, applied in the field of cresol production using molecular sieve as catalyst, can solve problems such as waste water and equipment corrosion

Active Publication Date: 2016-01-20
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

[0009] The technical problem to be solved by the present invention is that in the previous cresol production technology, equipment corrosion was serious and a large amount of waste water was produced in the production process. The present invention provides a method for producing cresol by phenol-methanol shape-selective catalysis

Method used

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  • A kind of method that takes molecular sieve as catalyst to produce cresol
  • A kind of method that takes molecular sieve as catalyst to produce cresol
  • A kind of method that takes molecular sieve as catalyst to produce cresol

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Experimental program
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Effect test

Embodiment 1

[0025] The preparation process of the catalyst is as follows: 120 grams of MCM-49 molecular sieve with a molar silicon-aluminum ratio of 20, 80 grams of titanium oxide, and an appropriate amount of 10% dilute nitric acid as extrusion aids are extruded. Dry at 120°C and bake at 550°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 500°C for 10 hours to prepare A1. Immerse 20 grams of A1 sample in ammonium dihydrogen phosphate aqueous solution for 12 hours, dry at 120°C, and bake at 700°C for 3 hours, P 2 o 5 The weight content is 3%, and A2 is prepared. Catalyst A was obtained by steaming 20 grams of A2 in a 100% steam atmosphere for 10 hours at a temperature of 300° C. and calcining at 550° C. for 3 hours. Molecular sieve content 60%.

Embodiment 2

[0027] The preparation process of the catalyst is as follows: 80 grams of MCM-49 molecular sieve with a molar silicon-aluminum ratio of 30 is mixed with 100 g of titanium dioxide weight 20% titanium sol, 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 1-3 mm to prepare columnar catalyst matrix B0. Add 50 ml of 10% nitric acid solution by weight 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. Immerse 20 grams of B1 sample in ammonium dihydrogen phosphate aqueous solution for 12 hours, dry at 120°C, and bake at 550°C for 10 hours, P 2 o 5 The weight content is 0.01%, and B2 is prepared. Catalyst B was obtained by steaming 20 grams of B2 in a 100% steam atmosphere for 2 hours at a temperature of 600° C. and roasting at 550° C. for 3 hours. The molecular sieve...

Embodiment 3

[0029] The preparation process of the catalyst is as follows: 200 grams of MCM-49 molecular sieve with a molar silicon-aluminum ratio of 80 is mixed with 30 grams of titanium dioxide and 100 grams of titanium dioxide with a weight of 20% titanium sol, and an appropriate amount of 10% dilute nitric acid is added as an extrusion aid for extrusion molding. Dry at 120°C and bake at 550°C for 4 hours. The above catalyst was cut into 1-3 mm to prepare columnar catalyst precursor C0. Add 50 ml of 10% nitric acid solution by weight to 20 grams of precursor catalyst C0, soak at room temperature for 24 hours. Dry at 120°C and bake at 600°C for 3 hours to obtain C1. 20 grams of C1 sample was impregnated with calcium nitrate aqueous solution for 24 hours, dried at 120°C, and roasted at 600°C for 3 hours. The weight percentage of calcium oxide in the catalyst was 0.1%, and C2 was obtained. Catalyst C was obtained by steaming 20 grams of C2 in a 100% steam atmosphere for 10 hours at a temp...

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Abstract

The invention relates to a method of producing methylphenol by using a molecular sieve as a catalyst. Raw materials, namely phenol and methanol, after being preheated are mixed with a diluent gas, pass continuously through a catalyst bed layer, 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 molecular sieve catalyst is prepared by modification using MCM-49 as an active component. The phenol and the methanol are used as the raw materials. The methylphenol selectivity can reach 94%, and the para-position selectivity can reach 50%. 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 with molecular sieve as a catalyst. Background technique [0002] There are three isomers of cresol, p-cresol, o-cresol and m-cresol. p-cresol is a colorless liquid or crystal with a special smell, corrosive and toxic, insoluble in water, easily soluble in toluene, ethanol and other organic solvents, widely used in antioxidants, dyes, medicines, pesticides, spices, etc. industry. 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 contains about 30% phenol, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/07C07C37/16
CPCC07C37/16C07C39/07
Inventor 王坤院杨淼刘琳徐云鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI