A kind of preparation method of antioxidant modified carbon nanotube/hydrogenated nitrile 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, and can solve the problem of few reports and inconvenience of large-scale promotion , many environmental protection issues and other issues, to achieve the effect of simple preparation process, good thermal and oxidative aging resistance, and reduced self-polymerization ability

Active Publication Date: 2018-04-10
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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  • A kind of preparation method of antioxidant modified carbon nanotube/hydrogenated nitrile rubber
  • A kind of preparation method of antioxidant modified carbon nanotube/hydrogenated nitrile rubber
  • A kind of preparation method of antioxidant modified carbon nanotube/hydrogenated nitrile rubber

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preparation example Construction

[0031] The preparation method of the 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) to the mixed acid, and carry out a high temperature reaction. The high temperature reaction temperature is 70-150°C, and the reaction time is 1-6h. The 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), the carbon nanotubes and antioxidant obtained in step (1) are 1:0.3-1 by mass ratio, above the melting point of the antioxidant, use a mechanical force field to mix, and react for 30-50min, Taking out the product, washing off the unreacted antioxid...

Embodiment 1

[0043] (1) Preparation of functional carbon nanotubes

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

[0045] 100 g of activated carbon nanotubes and 50 g of hindered phenol AO-80 were weighed and pre-mixed, and then mechanically mixed at 140 °C for 30 min in a Hack rheometer, and the product was taken out and cooled to room temperature. The cooled product was centr...

Embodiment 2

[0054] (1) Preparation of functional carbon nanotubes

[0055] 120 g of multi-walled carbon nanotubes were weighed, and 4500 mL of concentrated sulfuric acid and 1500 mL of concentrated nitric acid were placed in a 10L beaker, and the mixture was mechanically stirred for 30min. After the temperature in the flask was lowered to room temperature, the activated carbon nanotubes were centrifuged and washed with a large amount of distilled water until neutral, and then placed in a vacuum drying oven and dried at 80° C. for 24 hours. The mass concentrations of concentrated sulfuric acid and concentrated nitric acid were 98% and 68%, respectively.

[0056] 100 g of activated carbon nanotubes and 50 g of hindered phenolic AO-80 were weighed and pre-mixed, and then mechanically mixed at 150 °C for 50 min in a Hack rheometer, and the product was taken out and cooled to room temperature. The cooled product was centrifuged and washed with a large amount of DMF, and then continued to be w...

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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 preparation method of antioxidant modified carbon nanotubes / hydrogenated nitrile rubber, which belongs to aging-resistant hydrogenated nitrile butadiene rubber. rubber processing, Background technique [0002] Long-term use of rubber will cause the rubber to age, causing the rubber material to harden, become brittle, decrease in strength, and gradually lose its sealing performance. Exposing the rubber material to high temperature air for a long time will produce a serious thermo-oxidative aging reaction, which greatly shortens the service life of the rubber material. For the hydrogenated nitrile rubber that often works under the condition of thermal oxygen, it is particularly important to effectively prevent the aging reaction of thermal oxygen. Although the double bond saturation of hydrogenated ni...

Claims

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Application Information

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Patent Type & Authority Patents(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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