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Preparation method for polymerization-type asymmetric hindered phenol anti-oxidant resins

A technology of asymmetric hindered phenols and antioxidants, which is applied in the synthesis field of polymerized asymmetric hindered phenolic antioxidant resins, can solve the problems of poor antioxidant activity and thermal stability of antioxidants, synthesis process pollution, etc., and achieve Good anti-oxidation effect, simple and safe process, good extraction resistance effect

Inactive Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The technical problem to be solved is that the existing antioxidant has poor antioxidant activity and thermal stability, and the defects of serious pollution in the synthesis process

Method used

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  • Preparation method for polymerization-type asymmetric hindered phenol anti-oxidant resins
  • Preparation method for polymerization-type asymmetric hindered phenol anti-oxidant resins

Examples

Experimental program
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Effect test

Embodiment 1

[0018] In a 500ml reactor equipped with a stirrer, reflux condenser, feeding device and nitrogen protection device, add 80g toluene, 100g p-cresol, 18g strong acid resin catalyst, replace with nitrogen, heat to 83 ° C, drop Dicyclopentadiene 112g, dropwise time 60min, after dropwise addition, heat up to 105°C, after 3.5h reaction, add phosphoric acid 1.0g, alkylation catalyst 12g, reaction temperature 75°C, dropwise add methanol and isobutanol 32g of mixed raw materials with a ratio of 3:7, adding time for 40 minutes, reacting for 2 hours after the dropping, filtering to remove the resin catalyst after the reaction, washing with alkali and water until neutral, stripping with water vapor to remove oligomers, solvents and The unreacted raw materials were distilled to 218°C under reduced pressure, and 161 g of the product was obtained after cooling, and the calculated product yield was 87.98%. The product is a brown resin, its molecular weight is 770-850 as determined by GPC, and...

Embodiment 2

[0020] In a 500ml reactor equipped with a stirrer, reflux condenser, feeding device and nitrogen protection device, add 100g toluene, 100g p-cresol, 26g strong acid resin catalyst, replace with nitrogen, heat to 80°C, drop Dicyclopentadiene 140g, dropwise time 42min, after dropwise addition, heat up to 110°C, after 3.5h reaction, add phosphoric acid 1.2g, alkylation catalyst 20g, reaction temperature 80°C, dropwise add methanol and isobutanol 40g of mixed raw materials with a ratio of 3:7, adding time of 40 minutes, reacting for 2 hours after the dropping, filtering to remove the resin catalyst after the reaction, washing with alkali and water until neutral, stripping with water vapor to remove oligomers, solvents and The unreacted raw materials were distilled to 247°C under reduced pressure, and 177g of the product was obtained after cooling, and the calculated product yield was 90.36%. The product is a brown resin, its molecular weight determined by GPC is 860-970, and its s...

Embodiment 3

[0022] In a 500ml reactor equipped with a stirrer, reflux condenser, feeding device and nitrogen protection device, add 80g toluene, 100g p-cresol, 20g strong acid resin catalyst, replace with nitrogen, heat to 90°C, drop Dicyclopentadiene 117g, dropwise time 60min, after dropwise addition, heat up to 102°C, after reaction for 4h, add phosphoric acid 1.6g, alkylation catalyst 22g, reaction temperature 86°C, dropwise add ethanol and isobutanol molar ratio 36g of mixed raw materials of 5:5, the dropping time is 40min, the reaction is 2.5h after the dropwise addition, the resin catalyst is removed by filtration after the reaction is completed, and after alkali washing and water washing to neutrality, the oligomers, solvent and The unreacted raw material was distilled to 233°C under reduced pressure, and 173 g of the product was obtained after cooling, and the calculated product yield was 90.22%. The product is a brown resin with a molecular weight of 740-900 and a softening point...

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Abstract

Provided is a preparation method for polymerization-type asymmetric hindered phenol anti-oxidant resins. The preparation method comprises steps: with strong acid resins as catalysts, and benzene or cyclohexane as a solvent, p-methylphenol and dicyclopentadiene are subjected to a polymerization reaction to form phenol-type petroleum resins; the phenol-type petroleum resins, saturated alcohols with one to three carbons and isobutanol are subjected to an alkylation reaction to form polymerization-type asymmetric hindered phenol anti-oxidant resins in presence of phosphoric acid and an active component nickel-containing alumina catalyst; the alkylation reaction products are subjected to reduced pressure distillation to remove oligomers, the solvent and the unreacted raw materials to obtain polymerization-type asymmetric hindered phenol antioxidant resin products, and the yield is about 90%. The preparation method has obvious positive effects, through asymmetric substituent groups antioxidant effects are raised. Compared to traditional phenol antioxidants, the synthesized polymerization-type asymmetric hindered phenol antioxidant resins are advantaged by high antioxidant activity, high heat stability, extracting resistance, compatibility, non-toxic and environmentally friendly characteristics.

Description

technical field [0001] The present invention relates to the synthesis method of polymerized asymmetric hindered phenolic antioxidant resin, especially relates to the preparation of dicyclopentadiene, p-cresol, C1-C3 saturated alcohol and isobutanol through polymerization and alkylation reaction. Type asymmetric hindered phenolic antioxidant resin method. Background technique [0002] Antioxidants are a class of polymer additives that can effectively reduce the rate of autoxidation of plastic or rubber products and delay aging degradation, and their applications involve almost all polymer products. Since most polymers need to be heated at 220-350°C to be processed into products, traditional antioxidants are easy to volatilize at high temperatures, thus affecting the performance of products and causing environmental degradation. At present, the typical antioxidants are amines and phenols. Among them, amine antioxidants are mainly used in rubber due to their high toxicity, and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/17C07C37/16
CPCY02P20/52
Inventor 刘威廉谢家明黄勇祁正娟黄彩凤李莹
Owner CHINA PETROLEUM & CHEM CORP
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