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A kind of modification method of nano white carbon black

A nano-silica, modification technology, applied in the field of preparation of modified synthetic rubber filler nano-silica, can solve the problems of long reaction time, large dosage, complicated operation, etc.

Active Publication Date: 2019-11-08
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above methods have improved the dispersion of nano-silica particles and enhanced the compatibility with the rubber matrix, these methods still have certain limitations. Using graft polymer modification and inorganic material surface coating to modify nano When using silica, there are disadvantages such as long reaction time, high energy consumption, and complicated operation; while using coupling agent or surfactant to modify nano-silica, there are also large dosage, high production cost, and poor dispersion stability. Easy to reunite and other disadvantages

Method used

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  • A kind of modification method of nano white carbon black
  • A kind of modification method of nano white carbon black
  • A kind of modification method of nano white carbon black

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of monomer pre-emulsion: 100 parts of 1,3-hexadiene, 6 parts of sodium dodecylbenzenesulfonate, 160 parts of deionized water, 1.2 parts of sodium hydroxide, and 0.03 parts of ammonium persulfate Put it into a reactor, heat up to 45°C, stir and react for 40 minutes to prepare 1,3-hexadiene pre-emulsion a.

[0034] (2) Preparation of highly dispersed nano-silica: 100 parts of nano-silica (40nm) and 1.0 part of methacrylic acid (MAA), 200 parts of deionized water, and 1.0 part of sodium hydroxide are added to the polymerization kettle and stirred Mix for 20 minutes; then add 1.0 parts of sodium dodecylbenzenesulfonate and 5.5 parts of 1,3-hexadiene pre-emulsion a, stir and heat up to 65°C, and then stir and mix for 25 minutes to form nano-silica powder as the center The seeds of the composite emulsion; then add 60 parts of 1,3-hexadiene pre-emulsion a and 0.05 part of ammonium persulfate, after reacting for 3.0h, finally add 0.2 part of diethylhydroxylamine, ...

Embodiment 2

[0036] (1) Preparation of monomer pre-emulsion: same as Example 1.

[0037] (2) Preparation of highly dispersed nano-silica: 100 parts of nano-silica (40nm) and 2.0 parts of methacrylic acid (MAA), 250 parts of deionized water, and 1.5 parts of sodium hydroxide are added to the polymerization kettle and stirred Mix for 20 minutes; then add 2.5 parts of sodium dodecylbenzenesulfonate and 7 parts of 1,3-hexadiene pre-emulsion a, stir and heat up to 65°C, and then stir and mix for 25 minutes to form nano-silica powder as the center The seeds of the composite emulsion; then add 65 parts of 1,3-hexadiene pre-emulsion a and 0.09 part of ammonium persulfate, after reacting for 3.0h, finally add 0.2 part of diethylhydroxylamine, wash, dehydrate, dry, Grinding to obtain highly dispersed nano white carbon black. Sampling and analysis: standard samples were made, and the tested properties are shown in Table 1.

Embodiment 3

[0039] (1) Preparation of monomer pre-emulsion: 100 parts of 1,3-hexadiene, 8 parts of sodium dodecylbenzenesulfonate, 190 parts of deionized water, 1.4 parts of sodium hydroxide, and 0.05 parts of ammonium persulfate Put it into a reactor, heat up to 47°C, stir and react for 40 minutes to prepare 1,3-hexadiene pre-emulsion b.

[0040] (2) Preparation of highly dispersed nano-silica: 100 parts of nano-silica (40nm) and 3.0 parts of methacrylic acid (MAA), 270 parts of deionized water, and 2.5 parts of sodium hydroxide are added to the polymerization kettle and stirred Mix for 25 minutes; then add 3 parts of sodium dodecylbenzenesulfonate and 8.0 parts of 1,3-hexadiene pre-emulsion b, stir and heat up to 65°C, and then stir and mix for 25 minutes to form nano-silica powder as the center The seeds of the composite emulsion; then add 70 parts of 1,3-hexadiene pre-emulsion b and 0.11 parts of ammonium persulfate, after reacting for 3.0 hours, finally add 0.24 parts of diethylhydro...

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Abstract

The invention provides a modification method of highly dispersive white carbon black used as rubber filler. The highly dispersive white carbon black is prepared from an unsaturated carboxylic acid polar monomer and a conjugated diene monomer with an in-situ polymerization method. With adoption of the method, the problem of easy agglomeration of the nanometer white carbon black is solved, the nanometer white carbon black is endowed with super-dispersibility, and the method is simple to operate and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of modified synthetic rubber filler nano white carbon black. Background technique [0002] As we all know, from the perspective of the expected effect of inorganic powder filling modified rubber, the smaller the particle size of the inorganic powder particles, the better the effect of modification, but it is inevitable in the application process of ultrafine inorganic powder Encountered a technical problem, that is, as the particle size decreases, the specific surface area of ​​ultrafine powder increases, the surface energy increases, and the self-aggregation ability is stronger, so it is more difficult for the ultrafine powder to be mixed, infiltrated and dispersed by rubber materials. Therefore, the dispersion of ultrafine inorganic powder in rubber has become a bottleneck in the preparation of high-performance rubber materials. [0003] Nano-silica is a porous substance, and its composition can be SiO ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/04C08K3/36
CPCC08K3/36C08K9/08C08K2201/011
Inventor 徐典宏郭珺朱晶孟令坤蔡文婧丛日新张华强郑红兵王永峰燕鹏华
Owner PETROCHINA CO LTD
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