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Preparing method for antioxidant-modified carbon nano tube/hydrogenated butadiene-acrylonitrile rubber

A technology of hydrogenated nitrile rubber and carbon nanotubes, which is applied in the field of preparation of heat-resistant oxygen aging hydrogenated nitrile rubber, antioxidant modified carbon nanotubes/hydrogenated nitrile rubber, can solve the inconvenience of large-scale promotion, and is rarely reported , many environmental protection issues and other issues, to achieve good thermal oxygen aging resistance, simple preparation process, and reduce the effect of self-aggregation ability

Active Publication Date: 2016-10-12
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Few reports have been reported on carbon nanotubes with inert surfaces
At the same time, the main modification method is the liquid phase method, which has many environmental protection problems and is not convenient for large-scale promotion.

Method used

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  • Preparing method for antioxidant-modified carbon nano tube/hydrogenated butadiene-acrylonitrile rubber
  • Preparing method for antioxidant-modified carbon nano tube/hydrogenated butadiene-acrylonitrile rubber
  • Preparing method for antioxidant-modified carbon nano tube/hydrogenated butadiene-acrylonitrile rubber

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preparation example Construction

[0031] The preparation method of antioxidant modified carbon nanotube / hydrogenated nitrile rubber of the present invention specifically comprises the following steps:

[0032] (1) Mix concentrated sulfuric acid and concentrated nitric acid, add multi-walled carbon nanotubes (MWCNTS) into the mixed acid, and perform high-temperature reaction. The high-temperature reaction temperature is 70-150°C, and the reaction time is 1-6h. The final carbon nanotubes are washed with water until neutral and dried; wherein the volume ratio of concentrated sulfuric acid and concentrated nitric acid is one of 1:1, 2:1, 3:1 or 4:1. The washing method is one or more of centrifugal washing, suction filtration washing or vacuum distillation.

[0033](2), with the carbon nanotube and antioxidant that step (1) obtains, be 1:0.3-1 by mass ratio, above the fusing point of antioxidant, adopt mechanical force field to mix, and react 30-50min, The product is taken out, and the unreacted antioxidant is was...

Embodiment 1

[0043] (1) Preparation of functional carbon nanotubes

[0044] Weigh 120g of multi-walled carbon nanotubes, and simultaneously measure 4500mL of concentrated sulfuric acid and 1500mL of concentrated nitric acid into a 10L beaker, stir mechanically for 30min, transfer the mixture to a 10L three-necked flask, and reflux at 120°C for 3h. After the temperature in the flask dropped to room temperature, the activated carbon nanotubes were centrifuged and washed with a large amount of distilled water until neutral, and placed in a vacuum drying oven at 80° C. for 24 hours. The mass concentrations of concentrated sulfuric acid and concentrated nitric acid are 98% and 68% respectively.

[0045] Weigh 100 g of activated carbon nanotubes and 50 g of hindered phenol AO-80 for pre-mixing, then mechanically mix in a Haake rheometer at 140°C for 30 min, take out the product and cool to room temperature. The cooled product was centrifuged and washed with a large amount of DMF, and then conti...

Embodiment 2

[0054] (1) Preparation of functional carbon nanotubes

[0055] Weigh 120g of multi-walled carbon nanotubes, and simultaneously measure 4500mL of concentrated sulfuric acid and 1500mL of concentrated nitric acid into a 10L beaker, stir mechanically for 30min, transfer the mixture to a 10L three-necked flask, and reflux at 120°C for 1h. After the temperature in the flask dropped to room temperature, the activated carbon nanotubes were centrifuged and washed with a large amount of distilled water until neutral, and placed in a vacuum drying oven at 80° C. for 24 hours. The mass concentrations of concentrated sulfuric acid and concentrated nitric acid are 98% and 68% respectively.

[0056] Weigh 100 g of activated carbon nanotubes and 50 g of hindered phenol AO-80 for pre-mixing, mechanically mix in a Haake rheometer at 150°C for 50 min, take out the product and cool to room temperature. The cooled product was centrifuged and washed with a large amount of DMF, and then continued ...

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Abstract

The invention relates to a preparing method for antioxidant-modified carbon nano tube / hydrogenated butadiene-acrylonitrile rubber. The preparing method comprises the steps that firstly, a hindered phenol antioxidant is grafted to the surfaces of carbon nano tubes through a solid phase reaction from the angle of the molecular structure, then the antioxidant-modified carbon nano tube filler, hydrogenated butadiene-acrylonitrile rubber, a vulcanizing agent, an activating agent and a co-vulcanizing agent are mixed and vulcanized, and the product is obtained. The hydrogenated butadiene-acrylonitrile rubber prepared with the method has excellent mechanical properties, high-temperature resistance and hot oxygen aging resistance; besides, the antioxidant is not prone to self-aggregation and not likely to be separated from the rubber material, and thus the rubber product can have more stable performance; furthermore, no organic solvent is adopted, and environment friendliness of the preparing process is achieved.

Description

technical field [0001] The invention relates to a method for heat-resistant oxygen aging hydrogenated nitrile rubber filled with functional carbon nanotubes, in particular to a method for preparing antioxidant modified carbon nanotubes / hydrogenated nitrile rubber, which belongs to aging-resistant hydrogenated nitrile rubber processing field, Background technique [0002] Long-term use of rubber will cause the rubber to age, resulting in the hardening and brittleness of the rubber material, the decrease in strength, and the gradual loss of sealing performance. Exposing the rubber material to high temperature air for a long time will cause serious thermo-oxidative aging reaction, which will greatly shorten the service life of the rubber material. For hydrogenated nitrile rubber that often works under thermal oxygen conditions, it is particularly important to effectively prevent thermal oxygen aging reactions. Although the double bond saturation of hydrogenated nitrile rubber...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L15/00C08K13/06C08K9/04C08K9/02C08K7/24
CPCC08K7/24C08K9/02C08K9/04C08K13/06C08L2201/08C08L15/005
Inventor 张继华李杰李润源
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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