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Synthesis method of 2-methyl-6-tert-butylphenol

A technology of tert-butylphenol and a synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as only about 70%, and achieves reduction of residue discharge, high yield, and reduction of Effects of Environmental Pollution

Active Publication Date: 2013-06-19
PENGLAI HONGWEI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthetic method adopted by Ciba-Geigy Company is based on the synthetic method adopted in U.S. Patent U.S.P5098945. The catalyst is selected from ZSM zeolite or activated alumina, which is also a method of distillation under reduced pressure, but the yield can only be 70% about

Method used

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  • Synthesis method of 2-methyl-6-tert-butylphenol
  • Synthesis method of 2-methyl-6-tert-butylphenol

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1, synthetic 2-methyl-6-tert-butylphenol

[0021] In a 1000ml stainless steel autoclave, add 3.5mol of o-cresol and 0.105mol of anhydrous aluminum trichloride to seal the reactor, and perform nitrogen replacement. After nitrogen replacement, the autoclave is heated to 100°C, filled with 3.675mol of Keep the temperature of isobutene for 2 hours, then cool down the autoclave to room temperature, transfer the material to the acidification kettle, add 5g of concentrated sulfuric acid to neutralize, wash with water, distill under reduced pressure, and take the fraction at 98Kpa, 120-125°C.

[0022] After the distillation is complete, lower the temperature to 60°C, transfer the residue to a 500ml four-neck flask, add 80g toluene and 3.0g anhydrous aluminum trichloride to the 100g residue, and keep the temperature at 120°C for 20 hours, then cool down to Wash with water at 40°C for three times, dry and distill under reduced pressure to obtain the fraction at 95Kpa, ...

Embodiment 2

[0026] Embodiment 2, synthetic 2-methyl-6-tert-butylphenol

[0027] In a 1000ml stainless steel autoclave, add 3.5mol of o-cresol and 0.07mol of zinc dichloride to close the reactor, carry out nitrogen replacement, after the nitrogen replacement, the autoclave is heated to 90°C, filled with 3.64mol of isobutene, after filling the isobutene Keep the temperature for reaction for 2 hours, then cool the autoclave to room temperature, transfer the material to the acidification kettle, add 5g of concentrated sulfuric acid for neutralization, wash with water, distill under reduced pressure, and take the fraction at 95Kpa, 120-125°C.

[0028] After the distillation, the temperature was lowered to 50°C, and the residue was transferred to a 500ml four-neck flask, 100g of toluene and 3.0g of p-toluenesulfonic acid were added to the 100g of the residue, and the mixture was incubated at 130°C for 18 hours. Cool down to 50°C and wash with water three times, dry and then distill under reduce...

Embodiment 3

[0032] Embodiment 3, synthetic 2-methyl-6-tert-butylphenol

[0033] In a 1000ml stainless steel autoclave, add 3.5mol of o-cresol and 0.035mol of zinc dichloride to close the reactor, and perform nitrogen replacement. After the nitrogen replacement, the autoclave is heated to 100°C, filled with 3.5mol of isobutene, and then filled with isobutene Keep the temperature for reaction for 2 hours, then cool down the autoclave to room temperature, transfer the material to the acidification kettle, add 5g of concentrated sulfuric acid for neutralization, wash with water, distill under reduced pressure, and take the fraction at 98Kpa, 120-125°C.

[0034] After the distillation, the temperature was lowered to 50°C, and the residue was transferred to a 500ml four-necked flask, and 60g of toluene and 2.5g of titanium tetrachloride were added to 100g of the residue, and the reaction was carried out at 110°C for 20 hours. Lower the temperature to 50°C, wash with water three times, dry over ...

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Abstract

The invention discloses a synthesis method of 2-methyl-6-tert-butylphenol. The method comprises the following steps: 1) catalyzing raw materials o-cresol and isobutene with Lewis acid so as to react at the temperature of 80-130 DEG C, rectifying a reaction product I at the temperature of 95-98kPa, and collecting fraction with the temperature of 120-125 DEG C and kettle residue; 2) dissolving the kettle residue with an inert solvent, catalyzing with the Lewis acid, reacting at the temperature of 80-150 DEG C, rectifying a reaction product II at the temperature of 95-98 kPa, and collecting the fraction at the temperature of 120-125 DEG C; and 3) mixing the fractions collected in the steps 1) and 2) so as to obtain 2-methyl-6-tert-butylphenol. By using the synthesis method of the 2-methyl-6-tert-butylphenol, the yield of the product is high, the discharge of the residue is reduced, and the inert solvent in the reaction can be recycled after rectification and recovery, thereby reducing the environment pollution.

Description

technical field [0001] The invention relates to a method for synthesizing 2-methyl-6-tert-butylphenol. Background technique [0002] 2-Methyl-6-tert-butylphenol is a phenolic antioxidant and an important intermediate for the synthesis of high-grade hindered phenolic antioxidants such as Irganox245 and Sumilizer GA-80. At present, 2-methyl-6-tert-butylphenol is mainly synthesized from o-cresol and isobutylene under the action of catalysts. The catalysts currently used mainly include concentrated sulfuric acid, cation exchange resins, solid catalysts, etc., and their technologies have their own characteristics. , but its development trend is solid catalyst. The synthetic method adopted by Ciba-Geigy is based on the synthetic method adopted in U.S. Patent U.S.P5098945. The catalyst is ZSM zeolite or activated alumina, which is also a method of distillation under reduced pressure, but the yield can only be 70%. about. Contents of the invention [0003] The purpose of this i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/06C07C37/14
Inventor 王玉晓姚建文常加力王士君
Owner PENGLAI HONGWEI CHEM