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Preparation method of tert-butyl phenol

A technology for p-tert-butylphenol and isobutylene, which is applied in the field of preparation of tert-butylphenol, can solve the problems of strong catalyst corrosion, complicated process and operation, low reaction conversion rate, etc., and achieves stable catalyst activity, simple process and improved The effect of conversion rate

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

AI Technical Summary

Problems solved by technology

[0009] In view of the fact that in the prior art, isobutylene and p-cresol are used as raw materials to prepare 2,6-tert-butyl 4-methylphenol, the catalyst is highly corrosive, Environmental pollution, low reaction conversion rate, poor selectivity, complicated process and operation, etc., the invention provides a preparation method of tert-butylphenol

Method used

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  • Preparation method of tert-butyl phenol
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Examples

Experimental program
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Effect test

Embodiment 1

[0040] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 25% ZrOCl 2 ethanol solution, and then 30 g TiCl 4 dissolved in ZrOCl 2 In the ethanol solution, titrate with 20% ammonia water until there is no white precipitate, wash with deionized water for 5 times, each time for 10 minutes, the washing temperature is 40°C, wash until there is no chloride ion, and then put it in a vacuum at 90°C Dried in a drying oven for 6 hours, extruded and then calcined 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 o...

Embodiment 2

[0043] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 25% ZrOCl 2 ethanol solution, and then 35 g of TiCl 4 dissolved in ZrOCl 2 In the ethanol solution, titrate with 20% ammonia water until there is no white precipitate, wash with deionized water for 5 times, each time for 10 minutes, the washing temperature is 40°C, wash until there is no chloride ion, and then put it in a vacuum at 90°C Dried in a drying oven for 6 hours, extruded and then calcined 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 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 conditio...

Embodiment 3

[0046] (1) Preparation of solid superacid catalyst: a: 50 grams of ZrOCl 2 Dissolved in ethanol to obtain a mass concentration of 25% ZrOCl 2 ethanol solution, and then 35 g of TiCl 4 dissolved in ZrOCl 2 In the ethanol solution, titrate with 20% ammonia water until there is no white precipitate, wash with deionized water for 5 times, each time for 10 minutes, the washing temperature is 40°C, wash until there is no chloride ion, and then put it in a vacuum at 90°C Dried in a drying oven for 6 hours, extruded and then calcined 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 58°C, and the impregnation time is 6h; the decompression vacuum degree is 18000Pa; the ultrasonic vibration frequency is 58kHz, and then the solid particles are placed at 90°C Dry it in a vacuum oven for 6 hours under the conditio...

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Abstract

The invention discloses a preparation method of tert-butyl phenol. A fixed bed tubular reactor is adopted, a catalyst bed layer is arranged in the middle, a partition plate is arranged 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 a lower feeding section is arranged below a catalyst filling layer; isobutene and p-methylphenol are used as feedstock I and enter from a raw material inlet of the upper feeding section; isobutene and nitrogen are used as feedstock II to enter from a raw material inlet of the lower feeding section, the feedstock I is subjected to ammoniation reaction in the catalyst bed layer, a reacted material is mixed with the feedstock II from bottom to top for further reaction, and an obtained productis 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 increased, theupper-end feeding passes through the catalyst bed layer in a reciprocating manner, the reaction is more sufficient, and the conversion rate of isobutene is increased.

Description

technical field [0001] The invention relates to a method for preparing tert-butylphenol, in particular to a method for preparing 2,6-di-tert-butyl-4-methylphenol by using isobutylene 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 for synthetic ...

Claims

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Application Information

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IPC IPC(8): C07C37/14C07C39/06B01J27/055B01J37/03B01J37/02B01J37/34
CPCC07C37/14B01J27/055B01J37/031B01J37/0201B01J37/343C07C39/06
Inventor 刘野赵亮王岩于庆志党雷
Owner CHINA PETROLEUM & CHEM CORP
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