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Processing technique of 2,6-ditbutyl-4-methylphenol

A technology of methyl phenol and di-tert-butyl, which is applied in the production process field of 2.6-di-tert-butyl-4-methylphenol, and can solve the problems such as general purification effect

Inactive Publication Date: 2012-01-11
RUGAO JINLING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In addition, the traditional process adopts recrystallization or rectification process to establish independently, the purification effect is average, and the purity of the pure product is generally 98%.

Method used

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  • Processing technique of 2,6-ditbutyl-4-methylphenol
  • Processing technique of 2,6-ditbutyl-4-methylphenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 500 grams of p-cresol and 3 grams of methanesulfonic acid into a 1000ml four-necked flask equipped with a stirring tube, condenser tube, thermometer and isobutylene inlet tube. The temperature is raised to 70~72℃ under stirring, and isobutylene gas is slowly introduced to adjust The feeding speed is to ensure that there is no gas overflowing the reaction flask. After aeration time is about 8 hours, after sampling and detecting that the content of p-cresol is less than 5%, stop the aeration and keep it at this temperature for 2 hours to complete the alkylation reaction. 92.7% crude 2.6-di-tert-butyl-4-methylphenol. Then lower the temperature to below 30°C, slowly add 30% sodium hydroxide solution, adjust the pH to 7, add 500ml of water, stir for 2 hours, stand still, separate the water layer, introduce the organic phase into the rectifying flask, and reduce Pressure distillation, collect 988 grams of 158~162°C / 5mmHg fraction, add this fraction to a 2000ml reaction fla...

Embodiment 2

[0030] Add 500 grams of p-cresol and 6 grams of methanesulfonic acid to a 1000ml four-necked flask with a stirring tube, condenser tube, thermometer and isobutylene inlet tube. The temperature is raised to 78~80℃ under stirring, and isobutylene gas is slowly introduced to adjust The feeding speed is to ensure that there is no gas overflowing the reaction flask. After the aeration time is about 8 hours, after sampling and detecting that the p-cresol content is less than 5%, stop the aeration and keep it at this temperature for 2 hours. The alkylation reaction yield is 94.5. % Crude product of 2.6-di-tert-butyl-4-methylphenol. Then lower the temperature to below 30°C, slowly add 30% sodium hydroxide solution, adjust the pH to 7, add 800ml of water, stir for 2 hours, stand still, separate the water layer, introduce the organic phase into the distillation flask, and reduce Pressure distillation, collect 995 grams of 158~162℃ / 5mmHg fraction, add this fraction to a 2000ml reaction fl...

Embodiment 3

[0032] Add 500 grams of p-cresol and 3 grams of sulfamic acid into a 1000ml four-necked flask equipped with a stirring tube, condenser tube, thermometer and isobutylene inlet tube. The temperature is raised to 70-72°C while stirring, and isobutylene gas is slowly introduced. Enter the speed to ensure that there is no gas overflowing the reaction flask. After aeration time is about 8 hours, after sampling and detecting that the content of p-cresol is less than 5%, stop the aeration and keep it at this temperature for 2 hours. The alkylation reaction yield is 93.8%. The crude product of 2.6-di-tert-butyl-4-methylphenol. Then lower the temperature to below 30°C, slowly add 30% sodium hydroxide solution, adjust the pH to 7, add 500ml of water, stir for 2 hours, stand still, separate the water layer, introduce the organic phase into the rectifying flask, and reduce Pressure distillation, collect 990 grams of 158~162°C / 5mmHg fraction, add this fraction to a 2000ml reaction flask, add...

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Abstract

The invention mainly discloses a processing technique of 2,6-ditbutyl-4-methylphenol, which mainly comprises the steps of: alkylating methylphenol and isobutene and then neutralizing and washing the alkylated product. The processing technique of the 2,6-ditbutyl-4-methylphenol is characterized in that a catalyst with a usage amount of 0.3-1.5% mole percent of the methylphenol is added in the process of the alkylation of the methylphenol and the isobutene; the alkylated product after being washed is directed refined; methods of reduced pressure distillation and re-crystallization are jointly carried out in the refining process; and then the finished product of the 2,6-ditbutyl-4-methylphenol is obtained through offcentering and drying steps. The processing technique of the 2,6-ditbutyl-4-methylphenol has the advantages as follows: the yield of a course product of BHT (butylated hydroxytoluene) can reach 92% or higher with the adoption of methanesulfonic acid or sulfamic acid as a novel catalyst for the alkylation, and the purity of the pure product can reach 99% or higher through the joint of the reduced pressure distillation and the re-crystallization.

Description

Technical field [0001] The invention relates to a production process of 2.6-di-tert-butyl-4-methylphenol, in particular to a combined use of recrystallization and vacuum rectification procedures, and the use of a catalyst in the process to make the purity of the pure product Up to 99% or more. Background technique [0002] When the traditional 2.6-di-tert-butyl-4-methylphenol production process adopts the recrystallization method to obtain the finished product, the catalyst used is sulfuric acid, and the crude product of 2.6-di-tert-butyl-4-methylphenol is obtained by using this catalyst. The quality is about 85-90%, the yield is low, about 82%, and there are many side reactions, and the cost of raw materials is relatively high. In addition, because sulfuric acid is a strong acid, it is extremely corrosive to equipment and is not environmentally friendly. friendly. [0003] In addition, the traditional process adopts the recrystallization or rectification process to set up indepe...

Claims

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Application Information

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IPC IPC(8): C07C39/06C07C37/14C07C37/74C07C37/84
Inventor 王宏黄奎生黄雪平沈伟
Owner RUGAO JINLING CHEM
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