Method for producing methyl phenol

A technology of cresol and molecular sieve, which is applied in the field of cresol production, can solve problems such as waste water and equipment corrosion, reduce the temperature difference between inlet and outlet, ensure the safety and reliability of the process, and avoid by-products

Active Publication Date: 2014-07-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] According to the technical problem to be solved, the equipment corrosion in the previous cresol production technology was serious, and a large amount of waste water was generated in the production process. The present invention provides a method for producing cresol

Method used

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  • Method for producing methyl phenol

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Effect test

Embodiment 1

[0037] The preparation process of the molecular sieve catalyst is as follows: 170 grams of hydrogen-type MCM-22 molecular sieves with a molar silicon-aluminum ratio of 30 are mixed with 100 grams of silicon dioxide weight 30% silica sol, a certain amount of calcium acetate is added to mix evenly, and an appropriate amount of 10% Dilute nitric acid is used as extrusion aid to extrude into strips. 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 matrix A0. 20 grams of matrix catalyst A0 was added to 50 ml of nitric acid solution with a weight content of 10%, and soaked at room temperature for 12 hours. Dry at 120°C and bake at 500°C for 2 hours to prepare A1. Molecular sieve catalyst A was obtained by steaming 20 grams of Al in a 100% steam atmosphere for 10 hours at a temperature of 350° C. and roasting at 550° C. for 3 hours. The weight content of molecular sieve in the prepared catalyst is 85%, and the weight co...

Embodiment 2

[0039] The preparation process of the molecular sieve catalyst is as follows: 170 grams of hydrogen-type MCM-49 molecular sieves with a molar silicon-aluminum ratio of 28 are mixed with 100 grams of silicon dioxide weight 30% silica sol, a certain amount of barium calcium nitrate is added to mix evenly, and an appropriate amount of 10 % dilute nitric acid as extrusion aid, 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 matrix B0. 20 grams of matrix catalyst B0 was added to 50 ml of nitric acid solution with a weight content of 10%, and soaked at room temperature for 12 hours. B1 was prepared by drying at 120°C and calcining at 500°C for 2 hours. Molecular sieve catalyst B was obtained by steaming 20 grams of B1 in a 100% steam atmosphere for 4 hours at a temperature of 400° C. and roasting at 550° C. for 3 hours. The weight content of molecular sieve in the prepared catalyst is 85%, and the w...

Embodiment 3

[0041] The preparation process of the molecular sieve catalyst is as follows: 170 grams of ammonia-type ZSM-5 molecular sieve with a molar silicon-aluminum ratio of 80 is mixed with 100 grams of silicon dioxide weight 30% silica sol, a certain amount of lanthanum nitrate is added to mix evenly, and an appropriate amount of 10% Dilute nitric acid is used as extrusion aid to extrude into strips. 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 matrix C0. 20 grams of matrix catalyst C0 was added to 50 ml of nitric acid solution with a weight content of 10%, and soaked at room temperature for 12 hours. Dry at 120°C and bake at 500°C for 2 hours to obtain C1. Molecular sieve catalyst C was obtained by steaming 20 grams of C1 in a 100% steam atmosphere for 2 hours at a treatment temperature of 500° C. and roasting at 550° C. for 3 hours. The weight content of molecular sieve in the prepared catalyst is 85%, and the wei...

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Abstract

The present invention provides a process for the production of cresol. The raw materials comprising ethers, phenols and carbinol are preheated, and then continue through the multi-stage solid catalyst bed mixed with steam, carrying out a gas-phase reaction to product cresol at 250-450℃ reaction temperature, with 0.3-5h-1 feed weight airspeed, and under ordinary pressure. The solid catalyst is selected one or more from alumina, kaolin and molecular sieve catalyst. The phenols are selected from phenol, xylenol and mixture thereof. The ethers are selected from anisole, dimethyl ether, methylanisole, and their mixture of any two or more. When the once-through yield of cresol is 0.2g cresol/g catalyst, the para-selective of p-cresol could reach 45%. The catalyst has been characterized by excellent stability, and non-corrosiveness for equipment in productive process, which is a kind of environment-friendly catalyst with predictable industrial application prospect.

Description

technical field [0001] The present invention relates to a method for producing cresol. 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, and is widely used in antioxidants, dyes, medicines, pesticides, spices and other industries. O-cresol, also known as: 2-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, o-cresol 10%-13%, m-cresol 14%-18%, p-cresol 9%-12%, xylenol 13%-15%, traditional cresol The preparation method is a natural separation method, and the th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/07C07C37/16B01J29/70B01J29/40
CPCB01J8/04C07C39/07C07C37/11Y02P20/52C07C37/16B01J21/04B01J21/16B01J29/40B01J29/7007B01J29/7038B01J2229/36B01J2229/37
Inventor 王坤院徐云鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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