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Prepn process of 2,2'-methylene bis (4-methyl-6-tert-butyl phenol)

A technology of tert-butylphenol and methylene bis, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of strong corrosiveness, increase the post-processing process and preparation cost, and does not involve the stability of resin catalysts. Sexual issues etc.

Inactive Publication Date: 2004-06-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The acidic catalysts used in the document US4087469 include sulfuric acid, phosphoric acid and ion exchange resins, etc. When using sulfuric acid as a catalyst, the product after the reaction needs to be treated with alkali first, and then purified by distillation, which increases the post-treatment process and preparation cost of the reaction, and Strong corrosion; when ion exchange resin is used as catalyst, although the defect of liquid acid catalyst is overcome, it does not involve the stability of resin catalyst

Method used

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  • Prepn process of 2,2'-methylene bis (4-methyl-6-tert-butyl phenol)
  • Prepn process of 2,2'-methylene bis (4-methyl-6-tert-butyl phenol)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Resin catalyst:

[0022] Macroporous strongly acidic (-SOH) based on styrene-divinylbenzene copolymer 3 ) cation exchange resin, the exchange capacity is 4.3 milliequivalents / g, the average pore diameter of the resin is 205 angstroms, the resin is processed in a vacuum desiccator, the processing temperature is 90 ° C, and the processing time is 3 hours;

[0023] Add 217 milliliters of methylal, 100 grams of 2-tert-butyl-4-cresol (molar ratio 4:1) and 60 grams of the above-mentioned resin catalyst into a stainless steel reactor with stirring. After the reactor is sealed, open Stirrer, react at a reaction temperature of 70°C and a reaction time of 2.5 hours. After the reaction, the reaction product is cooled to room temperature, and the catalyst is separated by filtration. The filtrate is distilled to remove the solvent to obtain a crude reaction product, which is obtained by refining 2,2'-methylenebis(4-methyl-6-tert-butylphenol) product.

[0024] The yield of the prod...

Embodiment 2

[0027] Resin catalyst:

[0028] Macroporous strongly acidic (-SOH) based on styrene-divinylbenzene copolymer 3 ) a cation exchange resin with an exchange capacity of 4.8 milliequivalents / gram and an average resin pore diameter of 350 angstroms. The resin is treated in a vacuum desiccator at a treatment temperature of 105° C. and a treatment time of 2 hours;

[0029]Add 163 milliliters of methylal, 100 grams of 2-tert-butyl-4-cresol (molar ratio 3:1) and 50 grams of resin catalyst into a stainless steel reactor with stirring. After the reactor is sealed, start stirring device, reacted at a reaction temperature of 75° C. and a reaction time of 3 hours. After the reaction, the aftertreatment of the reaction product was the same as in Example 1.

[0030] The yield of the product is 98%, the melting point of the product is 129-130°C, and the purity of the product is 98%.

[0031] The separated resin catalyst was put back into the reactor, and the reaction was continued according ...

Embodiment 3

[0033] AmberlystXN-1005 strongly acidic (-SOH 3 ) Macroporous cation exchange resin with a resin exchange capacity of 3.5 milliequivalents / g and an average pore diameter of 80 angstroms. The resin is treated in a vacuum dryer at a treatment temperature of 100° C. and a treatment time of 2 hours;

[0034] Add 271 milliliters of methylal, 100 grams of 2-tert-butyl-4-cresol (molar ratio 5:1) and 50 grams of resin catalyst into a stainless steel reactor with stirring. After the reactor is sealed, start stirring device, reacted at a reaction temperature of 80° C. and a reaction time of 2 hours. After the reaction, the aftertreatment of the reaction product was the same as in Example 1.

[0035] The yield of the product is 85%, and the melting point of the product is 128-129°C.

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Abstract

The present invention relates to the preparation process of 2,2'-mehtylene bis(4-methyl-6-tert-butyl phenol). The present invention adopts macroporous strong acid cationic exchange resin, zeolite with SiO2 / Al2O3 molar ratio of 15-100, or heteropolyacid or other solid acid as catalyst; and formal and 2-tert-butyl-4-cresol as material, with the catalyst amount being 10-80 wt% of 2-tert-butyl-4-cresol. The reaction is performed at the temperature of 40-100 deg.c for 1-5 hr, and the reaction resultant is filtered, distilled and refined to obtain the product. The process of the present invention has the features of simple post-reaction treatment, high product yield, high product quality, no corrosion to the apparatus and high catalyst stability.

Description

technical field [0001] The invention relates to a method for preparing 2,2'-methylene bis(4-methyl-6-tert-butylphenol). Background technique [0002] 2,2'-Methylene bis (4-methyl-6-tert-butylphenol), the trade name is antioxidant 2246, the English name is: 2,2'-Methylenebis (4-methyl-6-tert- Butylphenol), molecular formula is: C 23 h 32 o 2 , is a general-purpose powerful bisphenol antioxidant. Antioxidant 2246 is a good non-polluting antioxidant, which has excellent inhibitory effects on aging caused by oxygen and heat and cracks caused by sunlight, and has high thermal stability, good anti-oxidation effect, and no pollution , no coloring, no frosting, good oil solubility, no volatilization loss, no effect on rubber vulcanization and plasticity, no destabilizing effect on latex, widely used in natural and various synthetic rubber, resin, polyethylene (PE) , polypropylene (PP), polyoxymethylene, chlorinated polyether, polyurethane and oth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/16C07C39/07
Inventor 乔建江张卫东张磊陈永福
Owner CHINA PETROLEUM & CHEM CORP
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