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Nano-silica immobilized hindered phenol antioxidant as well as preparation method and application of antioxidant

A technology of nano-silica and hindered phenols, which is applied in the field of antioxidants and can solve the problems of dark product color and limited application range

Inactive Publication Date: 2015-04-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, although some progress has been made in grafting antioxidant groups on the surface of nano-silica by using silane coupling agents, most of the antioxidant groups grafted on silica are amine groups, resulting in the The color of the product is darker, which limits its application range to a certain extent

Method used

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  • Nano-silica immobilized hindered phenol antioxidant as well as preparation method and application of antioxidant
  • Nano-silica immobilized hindered phenol antioxidant as well as preparation method and application of antioxidant
  • Nano-silica immobilized hindered phenol antioxidant as well as preparation method and application of antioxidant

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 20g of nano-silica with a particle size of 100nm to 100g of ethanol aqueous solution (75g of ethanol and 25g of water), and disperse by ultrasonic wave for 30min (ultrasonic frequency is 20kHz, power is 300W); then adjust the pH value to 4 with hydrochloric acid, and add 1g Silane coupling agent KH590, and stirred at a speed of 120rpm / min for 20min; heated to 70°C, stirred at a speed of 80rpm / min for 90min, then cooled to room temperature, filtered under reduced pressure, washed with ethanol and dried at 50°C After 12 hours, KH590 modified nano-silica was obtained. KH590 modified nano silica and 2g antioxidant GM (2‐tertbutyl‐6‐(3‐tertbutyl‐2‐hydroxy‐5‐cresylmethyl)‐4‐methylphenol acrylate, Guangzhou Synthetic Materials Research Institute Co., Ltd.) into 100g toluene, ultrasonically dispersed for 20min (ultrasonic frequency is 25kHz, power is 200W), heated to 80°C; 0.4g triethylamine was added, and reacted for 2h under stirring at 120rpm / min; After cooling to room ...

Embodiment 2

[0036] Add 40g of nano silicon dioxide with a particle size of 150nm to 160g of ethanol aqueous solution (120g of ethanol and 40g of water), ultrasonically disperse for 10min (ultrasonic frequency is 40kHz, power is 400W); then adjust the pH value to 5 with hydrochloric acid, add 5g Silane coupling agent KH590, and stirred at a speed of 160rpm / min for 15min; heated to 80°C, stirred at a speed of 120rpm / min for 60min, then cooled to room temperature, filtered under reduced pressure, washed with ethanol and dried at 80°C After 6 hours, KH590 modified nano-silica was obtained. Add KH590 modified nano-silica and 10g antioxidant GM to 150g toluene, ultrasonically disperse for 10min (ultrasonic frequency is 20kHz, power is 400W), heat up to 90°C; add 2.0g hexamethylenediamine, at 80rpm / min React for 1 h under the action of stirring; cool to room temperature, filter under reduced pressure, wash with toluene and ethanol respectively, and dry at 80°C for 6 h to obtain the nano-silica-i...

Embodiment 3

[0039] Add 30g of nano-silica with a particle size of 10nm to 80g of ethanol aqueous solution (60g of ethanol and 20g of water), and disperse by ultrasonic wave for 60min (ultrasonic frequency is 20kHz, power is 40W); then adjust the pH value to 4 with hydrochloric acid, and add 4g Silane coupling agent KH590, and stirred at a speed of 80rpm / min for 20min; heated to 50°C, stirred at a speed of 110rpm / min for 80min, then cooled to room temperature, filtered under reduced pressure, washed with ethanol and dried at 70°C After 8 hours, KH590 modified nano-silica was obtained. Add KH590 modified nano-silica and 9g antioxidant GM to 120g toluene, ultrasonically disperse for 15min (ultrasonic frequency is 30kHz, power is 300W), heat up to 60°C; add 1.0g diethylenetriamine, at 100rpm / React for 3 hours under stirring for 1 min; cool to room temperature, filter under reduced pressure, wash with toluene and ethanol respectively, and dry at 70°C for 8 hours to obtain the nano-silica-immo...

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Abstract

The invention discloses a nano-silica immobilized hindered phenol antioxidant as well as a preparation method and an application of the antioxidant. According to the preparation method, ethanol water is taken as a dispersion medium, a silane coupling agent kh590 is hydrolyzed to generate hydroxyls which join in condensation polymerization with the hydroxyls of nano-silica, and then the KH590 modified nano-silica containing the sulfydryl can be obtained after suction filtration, washing and drying; under the action of ultrasonic, the KH590 modified nano-silica and the hindered phenol antioxidant GM are dispersed into toluene; under the action of a catalyst, the sulfydryl reactions with the double bond C=C of the GM, and finally, the nano-silica immobilized hindered phenol antioxidant can be obtained after suction filtration, washing and drying. The suction filtration, washing and drying prepared is capable of overcoming the defects of poor extraction resistance of a traditional small molecular antioxidant and also advantageous for improving the mechanical properties of a matrix material, and can be widely applied to natural rubber, butadiene rubber and butadiene styrene rubber.

Description

technical field [0001] The invention relates to the field of antioxidants, in particular to a nano-silica immobilized hindered phenolic antioxidant and a preparation method and application thereof. Background technique [0002] Antioxidants are a kind of additives widely used in polymer materials, especially rubber, which can effectively inhibit the occurrence of aging phenomena and prolong their service life. Currently commonly used antioxidants are hindered phenolic and amine antioxidants. However, traditional antioxidants have a small molecular weight, generally below 500, so they are easy to volatilize and migrate during the processing and use of rubber, and have poor extraction resistance, which will lead to a decrease in the antioxidant capacity of rubber and its products and a longer service life. shorten. Therefore, how to improve the antioxidant efficiency of antioxidants in rubber has become one of the hotspots of research in recent years. As an inorganic filler...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/12C08K5/134C08K9/06C08K3/36C08L7/00C08L9/00C08L9/06C08K13/06C08J3/24
Inventor 李红强曾幸荣赖学军李峰吴文剑
Owner SOUTH CHINA UNIV OF TECH
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