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Method for preparing tert-butyl phenol

A technology of tert-butylphenol and catalyst bed, which is applied in chemical instruments and methods, preparation of organic compounds, production of bulk chemicals, etc. It can solve problems such as strong catalyst corrosion, complicated process and operation, and low reaction conversion rate , to achieve the effect of stable catalyst activity, simple process and improved conversion rate

Active Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the method for preparing 2,6-tert-butyl 4-methylphenol in the prior art using MTBE and p-cresol as raw materials, the catalyst is highly corrosive, pollutes the environment, the reaction conversion rate is low, the selectivity is poor, and the process and operation Complicated problems, the invention provides a method for preparing tert-butylphenol

Method used

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  • Method for preparing tert-butyl phenol
  • Method for preparing tert-butyl phenol

Examples

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Comparison scheme
Effect test

Embodiment 1

[0039] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 30% ZrOCl 2 Ethanol solution, titrated with 20% ammonia water until there is no white precipitate, washed 5 times with deionized water, 10 minutes each time, washing temperature is 40 ° C, washed to no chloride ion, and then placed in vacuum drying at 90 ° C Dry in an oven for 6 hours, extrude and then bake at 500°C for 8 hours to obtain white solid particles for use. b: impregnate the white particles obtained in step 1 with a silver nitrate sulfuric acid solution with a concentration of 2mol / L, the impregnation temperature is 55°C, and the impregnation time is 6h; the decompression vacuum degree is 15000Pa; the ultrasonic vibration frequency is 55kHz, and then the solid particles are placed at 90°C Dry it in a vacuum oven for 6 hours under the condition of 500°C for 8 hours to obtain the particle I. c: Repeat the impregnation process of step 2 wi...

Embodiment 2

[0042] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 35% ZrOCl 2 Ethanol solution, titrated with 20% ammonia water until there is no white precipitate, washed 5 times with deionized water, 10 minutes each time, washing temperature is 40 ° C, washed to no chloride ion, and then placed in vacuum drying at 90 ° C Dry in an oven for 6 hours, extrude and then bake at 500°C for 8 hours to obtain white solid particles for use. b: Impregnate the white particles obtained in step 1 with a silver nitrate sulfuric acid solution with a concentration of 3mol / L, the impregnation temperature is 58°C, and the impregnation time is 6h; the decompression vacuum degree is 16000Pa; the ultrasonic vibration frequency is 55kHz, and then the solid particles are placed at 90°C Dry it in a vacuum oven for 6 hours under the condition of 500°C for 8 hours to obtain the particle I. c: Repeat the impregnation process of step 2 wi...

Embodiment 3

[0045] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 35% ZrOCl 2 Ethanol solution, titrated with 20% ammonia water until there is no white precipitate, washed 5 times with deionized water, 10 minutes each time, washing temperature is 40 ° C, washed to no chloride ion, and then placed in vacuum drying at 90 ° C Dry in an oven for 6 hours, extrude and then bake at 500°C for 8 hours to obtain white solid particles for use. b: impregnate the white particles obtained in step 1 with a silver nitrate sulfuric acid solution with a concentration of 2mol / L, the impregnation temperature is 57°C, and the impregnation time is 6h; the decompression vacuum degree is 18000Pa; the ultrasonic vibration frequency is 55kHz, and then the solid particles are placed at 90°C Dry it in a vacuum oven for 6 hours under the condition of 500°C for 8 hours to obtain the particle I. c: Repeat the impregnation process of step 2 wi...

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Abstract

The invention discloses a method for preparing tert-butyl phenol. According to the method, a fixed bed tubular reactor is adopted, a catalyst bed layer is arranged in the middle, a partition plate isarranged at the upper part in the axial direction, the lower end of the partition plate extends into the catalyst bed layer and incompletely penetrates through the catalyst bed layer, the reactor is divided into three parts, an upper feeding section and a discharging section are arranged on two sides of the partition plate, and the part below a catalyst filling layer is a lower feeding section; MTBE and p-methylphenol are used as feedstock I and are enabled to enter from a raw material inlet of the upper feeding section; MTBE and nitrogen are used as feedstock II and are enabled to enter froma raw material inlet of the lower feeding section, the feedstock I is reacted in the catalyst bed layer, an obtained reacted material is mixed with the feedstock II from bottom to top for further reaction, and an obtained product is discharged from a discharge port of the discharging section. According to the reaction mode of the method, the material reaction is more sufficient, the reaction conversion rate is improved, the upper end feeding passes through the catalyst bed layer in a reciprocating manner, the reaction is more sufficient, and the conversion rate of MTBE is improved.

Description

technical field [0001] The invention relates to a method for preparing tert-butylphenol, especially a method for preparing 2,6-di-tert-butyl-4-methylphenol by using MTBE (methyl tert-butyl ether) and p-cresol as raw materials. Background technique [0002] 2,6-di-tert-butyl-4-methylphenol is white or light yellow crystal, and its molecular formula is C 15 h 24 O. Soluble in toluene, soluble in acetone, ethanol, benzene, ether, isopropanol, methanol, 2-butanone, ethylene glycol ethyl ether, petroleum ether and other organic solutions, insoluble in water and alkaline solutions. 2,6-tert-butyl 4-methylphenol is a general-purpose antioxidant, mainly used as an antioxidant additive for various petroleum products, as an antioxidant and stabilizer for some polymer materials, and as a food Antioxidant in the processing industry, also a phenolic antiaging agent for rubber, widely used in natural rubber, various synthetic rubber and its latex, and can also be used as a stabilizer f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/11C07C39/06B01J8/22B01J8/00
CPCC07C37/11B01J8/22B01J8/0085B01J8/0025C07C39/06Y02P20/52
Inventor 刘野赵亮王岩于庆志党雷
Owner CHINA PETROLEUM & CHEM CORP
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