Preparation method of nano-silica surface grafted hydroxyl terminated polybutadiene rubber

A technology of hydroxyl-terminated polybutadiene and nano-silica, which is applied in the treatment of dyed low-molecular organic compounds, dyed high-molecular organic compounds, and fibrous fillers. It can solve the problem of low grafting amount and achieve enhanced mechanical properties. Performance, simple reaction synthesis process, and improved dispersibility

Active Publication Date: 2015-10-07
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Generally, the surface of silica is modified by small molecule modifiers, such as Tan Xiumin 1 et al. modified the surface of nano-silica with a silane coupling agent, but the amount of grafting was low, and the agglomeration of nano-silica did not change significantly after modification.

Method used

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  • Preparation method of nano-silica surface grafted hydroxyl terminated polybutadiene rubber
  • Preparation method of nano-silica surface grafted hydroxyl terminated polybutadiene rubber
  • Preparation method of nano-silica surface grafted hydroxyl terminated polybutadiene rubber

Examples

Experimental program
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Effect test

Embodiment 1

[0021] 1) Synthesis of isocyanate-terminated nano-silica: first clean and activate the nano-silica, take 5 g of the activated nano-silica and put it into a 250 ml three-necked flask equipped with a stirring bar and a reflux condenser, then add 150 ml of acetone solution , ultrasonic dispersion for 30 minutes. Under an inert atmosphere, slowly drop a mixed solution containing 0.005g of the catalyst dibutyltin dilaurate and 5g of isophorone diisocyanate, react at 50°C for 6 hours, collect by centrifugation, and use acetone to ultrasonically disperse and wash and centrifuge three times to obtain Nano silica with isocyanate groups on the surface;

[0022] (2) Synthesis of modified nano-silica on the surface of hydroxyl-terminated polybutadiene rubber: get 5 g of nano-silica with isocyanate groups on the surface synthesized in (2) and pack into 250 ml with stirring Then add 150ml of butyl acetate solution to the three-necked flask with the reflux condenser, and ultrasonically disp...

Embodiment 2

[0025] (1) Synthesis of isocyanate-terminated nano-silica: first clean and activate the nano-silica, take 5g of the activated nano-silica and put it into a 250ml three-necked flask equipped with a stirring bar and a reflux condenser, then add 150ml of acetone solution, ultrasonically dispersed for 40 minutes. Under an inert atmosphere, slowly drop a mixed solution containing 0.03 g of the catalyst stannous octoate and 10 g of isophorone diisocyanate, react at 60 ° C for 5 hours, collect by centrifugation, and use acetone to ultrasonically disperse and wash and centrifuge four times to obtain the surface Nano silica containing isocyanate groups;

[0026] (2) Synthesis of modified nano-silica on the surface of hydroxyl-terminated polybutadiene rubber: get 5 g of nano-silica with isocyanate groups on the surface synthesized in (2) and pack into 250 ml with stirring Then add 150ml of butyl acetate solution to the three-necked flask with the reflux condenser, and ultrasonically di...

Embodiment 3

[0028] (1) Synthesis of isocyanate-terminated nano-silica: first clean and activate the nano-silica, take 5g of the activated nano-silica and put it into a 250ml three-necked flask equipped with a stirring bar and a reflux condenser, then add 150ml of acetone solution, ultrasonically dispersed for 50 minutes. Under an inert atmosphere, slowly drop a mixed solution containing 0.1 g of catalyst bis(dodecylsulfur) dibutyltin and 15 g of isophorone diisocyanate, react at 80°C for 3 hours, collect by centrifugation, and disperse with acetone ultrasonically Wash and centrifuge five times to obtain nano-silica containing isocyanate groups on the surface;

[0029] (2) Synthesis of modified nano-silica on the surface of hydroxyl-terminated polybutadiene rubber: get 5 g of nano-silica with isocyanate groups on the surface synthesized in (2) and pack into 250 ml with stirring Then add 150ml of butyl acetate solution to the three-necked flask with the reflux condenser, and ultrasonically...

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Abstract

The invention discloses a preparation method of a nano-silica surface grafted hydroxyl terminated polybutadiene rubber. The method includes: 1) synthesis of isocyanate terminated nano-silica: dispersing cleaned and activated nano-silica into an acetone solution, conducting ultrasonic dispersion for dozens of minutes, slowly adding a catalyst containing isophorone diisocyanate solution dropwise according to the mass ratio of nano-silica to isophorone diisocyanate of 1:1-3, carrying out reaction at 50-80DEG C for 3-6h, performing centrifugal collection, then using acetone to conduct ultrasonic dispersing, washing and centrifugation three to five times, thus obtaining nano-silica with surface containing an isocyanic acid group; and 2) synthesis of hydroxyl terminated polybutadiene rubber surface grafted modified nano-silica. The modified nano-silica has good dispersibility in butyl acetate solution, and the surface polymer grafting content is high.

Description

1. Technical field [0001] The invention relates to a preparation method of polybutadiene rubber grafted with hydroxyl end on the surface of nano silicon dioxide, which belongs to the field of nano composite materials. 2. Background technology [0002] In recent years, organic / inorganic nanocomposites will bring special changes to the physical and chemical properties of materials due to their dispersed phase size in the transition region between macro and micro, with excellent mechanical properties, thermal stability and special Surface properties, etc., are increasingly concerned. Among many inorganic nanomaterials, nano-silicon dioxide has been widely concerned by researchers because of its high thermal stability, non-toxicity, good dielectric properties, and commercialization. In addition, nano-silica can also greatly improve the mechanical strength, toughness, wear resistance and aging resistance of polymer materials, so it has many applications in electronics, chemical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/28C09C3/08C09C3/10C08K9/06
Inventor 李加鹏胡柏星何其慧顾思云
Owner NANJING UNIV
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