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Preparation method of epoxidized natural rubber masterbatch with highly dispersed nano-silicon dioxide/carbon black

A technology of nano-silica and natural rubber, which is applied in the field of preparation of nano-silica and carbon black highly dispersed in epoxidized natural rubber masterbatch, which can solve the problem of poor wear resistance, low surface wettability, and inability to achieve Green tire requirements and other issues, to achieve the effect of simple process and easy large-scale production

Inactive Publication Date: 2011-06-29
AGRI PRODS PROCESSING RES INST CHINESE ACAD OF TROPICAL AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ENR has poor mechanical properties, especially poor wear resistance, so it is necessary to find a suitable filler system to fill and reinforce it, so as to achieve the purpose of preparing tires.
[0003] Carbon black is the traditional reinforcing filler for preparing tires. However, tires filled only with carbon black can no longer meet the requirements of today's low-carbon society for green tires.
It is an indisputable fact that the tires prepared by filling reinforced rubber with nano-silica can improve the grip on wet roads and reduce the rolling resistance of the tread, which is in line with the fact that green tires are prepared, but their wear resistance has not yet reached the level of carbon black-filled reinforced tires. Therefore, nano-silica cannot completely replace carbon black filled rubber to prepare tires. Using the synergistic effect of nano-silica and carbon black, the filled rubber can be reinforced and meets the purpose of green tires.
However, the surface interaction energy of nano-silica particles is strong, and they are easy to agglomerate to form an aggregated structure; carbon black always exists in the form of aggregates, and the surface wettability is low, resulting in poor dispersion performance
Commonly used reinforcing agents such as nano-silica and carbon black are added in the state of dry rubber. During the mixing process, it is difficult for the rubber to "eat powder", and the powder is flying, which pollutes the environment and seriously endangers the health of the operators. The strong agent is not well dispersed in the rubber, especially the nano-reinforced agent is easy to agglomerate in the rubber, which seriously affects the reinforcing effect

Method used

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  • Preparation method of epoxidized natural rubber masterbatch with highly dispersed nano-silicon dioxide/carbon black
  • Preparation method of epoxidized natural rubber masterbatch with highly dispersed nano-silicon dioxide/carbon black
  • Preparation method of epoxidized natural rubber masterbatch with highly dispersed nano-silicon dioxide/carbon black

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Experimental program
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Effect test

Embodiment 1

[0030] a. Nano-silica modification: Measure 20 parts of Si69, add 72 mL of absolute ethanol and 8 mL of deionized water, and adjust the pH to 8-9 with 0.01 part of triethylamine at the same time, add to the weighed 5 Parts of gas-phase method nano-silica, stirred and reacted for 24 hours, then centrifuged, washed, and freeze-dried to obtain modified nano-silica, which is ready for use.

[0031] b. Modification of carbon black: Weigh 5 parts of N330, add 100 mL of deionized water, ultrasonically disperse, add 10 parts of oxidant ammonium persulfate at the same time, stir for 36 hours, centrifuge, wash, and freeze-dry to obtain oxidation modification carbon black, spare.

[0032] c. Weigh 5 parts of the modified nano-silica obtained in (a) and the modified carbon black obtained in 5 parts of (b), add them into 100 mL of deionized water respectively, disperse them ultrasonically for 5 minutes, and add them to 100 parts of epoxy resins with an epoxy degree of 25%. , in epoxidized...

Embodiment 2

[0037] a. Nano-silica modification: Measure 20 parts of KH560, add 72 mL of absolute ethanol and 8 mL of deionized water, and at the same time adjust the pH to 8-9 with 0.01 part of triethylamine, and add it to the weighed 5 Parts of nano-silica by precipitation method, stirred and reacted for 24 hours, centrifuged, washed, and freeze-dried to obtain modified nano-silica, which was set aside.

[0038] b. Modification of carbon black: Weigh 5 parts of N220, add 100 mL of deionized water, ultrasonically disperse, and add 10 parts of oxidant hydrogen peroxide at the same time, stir and react for 36 hours, centrifuge, wash, and freeze-dry to obtain oxidation modification carbon black, spare.

[0039] c. Weigh 5 parts of the modified nano-silica obtained in (a) and 5 parts of the modified carbon black obtained in (b), add them into 100mL deionized water respectively, disperse them ultrasonically for 5min, and add them to 100 parts of epoxy degree 40% , in epoxidized natural rubber...

Embodiment 3

[0044] a. Nano-silica modification: Measure 20 parts of A151, add 72 mL of absolute ethanol and 8 mL of deionized water, and at the same time adjust the pH to 8-9 with 0.01 part of triethylamine. After hydrolysis for 1 hour, add to the weighed 5 Parts of gas-phase nano-silica, stirred and reacted for 24 hours, centrifuged, washed, and freeze-dried to obtain modified nano-silica, which was set aside.

[0045] b. Modification of carbon black: Weigh 5 parts of N375, add 100 mL of deionized water, ultrasonically disperse, add 10 parts of ammonium persulfate at the same time, centrifuge, wash and freeze-dry after stirring for 36 hours to obtain oxidatively modified Carbon black, spare.

[0046] c. Weigh 5 parts of the modified nano-silica obtained in (a) and 5 parts of the modified carbon black obtained in (b), add them into 100mL of deionized water respectively, disperse by ultrasonic for 5min, and add to 100 parts of epoxy degree 50% , in epoxidized natural rubber latex with a s...

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Abstract

The invention discloses a preparation method of an epoxidized natural rubber masterbatch with highly dispersed nano-silicon dioxide / carbon black, which comprises the following steps: performing ultrasonic dispersion on nano-silicon dioxide modified by a silane coupling agent and carbon block after liquid phase oxidation by an oxidant by using deionized water, then adding the nano-silicon dioxide into epoxidized natural rubber latex, stirring, finally performing steam solidification or solidification by a solidifying agent, drying, and getting the epoxidized natural rubber masterbatch with the highly dispersed nano-silicon dioxide / carbon black. Compared with the mechanical properties of the masterbatch prepared by adding the same parts of the nano-silicon dioxide / carbon black powder, the mechanical properties of the masterbatch are as follows: the 100% modulus is improved from 2.3MPa to 3.1-3.4MPa, the 300% modulus is improved from 9.2MPa to 10.1-11.6MPa, the tensile strength is improved from 31.2MPa to 33.5-36.8 MPa, the elongation at break is improved from 625% to 647%-688%, and the tearing strength is improved from 48.3N / mm to 53.8-58.3N / mm; furthermore, the process is simple, and the large-scale production is easy.

Description

【Technical field】 [0001] The invention relates to a method for preparing a master batch, in particular to a method for preparing a nano-silica and carbon black highly dispersed in an epoxidized natural rubber master batch. 【Background technique】 [0002] Epoxidized natural rubber (ENR) is made by chemically modifying natural rubber (NR) and attaching epoxy groups to the double bonds of the rubber molecular chain. Due to the introduction of epoxy groups, the polarity of the rubber molecules Increase, the force between molecules is strengthened, so that ENR has many unique properties, excellent air tightness, good oil resistance, good adhesion with other materials, especially when made into tire tread rubber , high wet road grip and low rolling resistance, the two properties are perfectly combined on the tire tread, therefore, ENR has a wide application prospect in the preparation of green tires. However, ENR has poor mechanical properties, especially poor wear resistance, so...

Claims

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Application Information

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IPC IPC(8): C08L15/00C08K9/06C08K3/36C08K9/02C08K3/04C08C1/14
Inventor 彭政黄田富罗勇悦汪月琼钟杰平李永振廖双泉
Owner AGRI PRODS PROCESSING RES INST CHINESE ACAD OF TROPICAL AGRI SCI
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