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Nano-silica/poly(conjugated diene) composite emulsion and preparation method thereof

A technology of nano-silica and polyconjugated diene, which is applied in the field of preparation of functional emulsions, can solve the problems of narrow PSN molecular weight distribution, difficulty in processing and application, and quality loss, and achieves simple and easy control of the preparation process, low cost, and improved The effect of overall performance

Active Publication Date: 2012-10-17
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because polybutadiene / silica composites are prepared by solution polymerization using n-butyllithium as an initiator, a large amount of organic solvents are used in the preparation process, which is not only harmful to the environment, but also macromolecules It is difficult for the chain to contain and coagulate all the silica particles, and there will be a loss of quality. At the same time, it may also aggregate in the co-coagulation gel matrix, making it difficult to achieve good dispersion
In addition, the PSN prepared by the solution polymerization method has a narrow molecular weight distribution, and there are certain difficulties in the application process of rubber post-processing

Method used

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  • Nano-silica/poly(conjugated diene) composite emulsion and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0034] a) Surface functional modification of nano-silica: Weigh 120g of nano-silica and dry it in an oven for use, then mix it with 1200g of toluene and then ultrasonically disperse it fully. hours, then filtered, washed, and vacuum-dried.

[0035] b) Preparation of functional emulsion

[0036] The first step is the preparation of monomer pre-emulsion. 1,200 g of 1,3-butadiene, 120 g of sodium dodecylbenzenesulfonate, 1,800 g of deionized water, 12 g of sodium hydroxide, and 2.4 g of potassium persulfate were mixed and pre-emulsified for 20 minutes to prepare a pre-emulsion.

[0037] In the second step, the functional emulsion is prepared with the modified nano-silica as the core. Take 3.6g of nano-silica modified by surface functionalization and add it to a reactor containing 60g sodium dodecylbenzenesulfonate and 480g deionized water, stir and heat up to 60°C, and then take 313g monomer pre-emulsion Add it into the reactor, control the temperature of the reactor at 60°C, ...

Embodiment 2

[0039] a) According to the method disclosed in "Journal of Radiation Research and Radiation Technology", Volume 25, No. 5, "Study on Surface Modification of Nano-Silicon Dioxide and Radiation-Initiated Grafting GMA" in 2007, prepare surface-functionalized modified nano-silicon dioxide Method: Weigh 6g of nano-silicon dioxide and dry it in an oven at 50°C for 5 hours, add the dried nano-silicon dioxide to an aqueous solution in which 96g of coupling agent MPS is dissolved, and disperse it ultrasonically for 1 hour. After dispersion, the mixture was stirred at 110°C for 8h. After filtration, the modified silicon dioxide was washed with toluene, and the obtained product was vacuum filtered, extracted by Soxhlet, and finally dried in an oven.

[0040] b) Preparation of functional emulsion

[0041] The first step is the preparation of monomer pre-emulsion. 1200 g of isoprene, 72 g of sodium lauryl sulfate, 1200 g of deionized water, 6 g of ammonia water, and 9.6 g of ammonium per...

Embodiment 3

[0044] a) Surface functional modification of nano-silica: Weigh 240g of nano-silica and dry it in an oven for use, then mix it with 4800g of xylene and then ultrasonically disperse it fully, add 312g of hydrolyzed VTMS, stir and heat to 93°C for reflux 4 hours, then filtered, washed, and vacuum dried.

[0045] b) Preparation of functional emulsion

[0046] The first step is the preparation of monomer pre-emulsion. Prepare by mixing 1200g of 1,3-pentadiene, 40g of sodium dodecylbenzenesulfonate, 200g of alkylphenol polyoxyethylene ether, 1920g of deionized water, 9.6g of sodium carbonate and 9.8g of sodium persulfate for 30 minutes into a pre-emulsion.

[0047] In the second step, the functional emulsion is prepared with the modified nano-silica as the core. Get 54g of surface-functionalized modified nano-silica and add it to a reactor equipped with 54g fatty acid soap and 456g deionized water, stir and heat up to 68°C, then get 676g monomer pre-emulsion and add it to the re...

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Abstract

The invention discloses a nano-silica / poly(conjugated diene) composite emulsion and a preparation method thereof. Based on emulsion dry basis, the nano-silica / poly(conjugated diene) composite emulsion comprises 0.1 to 5 parts of surface functionalization-modified nano-silica. The nano-silica / poly(conjugated diene) composite emulsion has granularity of 50 to 80nm, number-average molecular weight of 100000 to 120000, and molecular weight distribution of 2 to 3. The invention also discloses the preparation method of the nano-silica / poly(conjugated diene) composite emulsion.

Description

technical field [0001] The invention relates to a preparation method of a functional emulsion used for rubber modification, and more specifically relates to a preparation method of a nano-silica / polyconjugated diene composite emulsion. Background technique [0002] With the development of automobiles in the direction of high speed, safety, energy saving and comfort, the requirements for high performance tires are also increasing year by year, which requires tire treads to have good wet skid resistance, excellent wear resistance and low rolling resistance. [0003] Nano-silica, commonly known as white carbon black, is the second largest reinforcing agent in the rubber industry after carbon black, and is widely used in tire tread formulations. In recent years, with the application and development of modern electron microscopy and computer science, people have gradually researched and developed silicon dioxide from the perspective of microscopic particles, and prepared polymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L9/00C08K9/06C08K3/36C08F36/04C08F2/44C08F2/24C08L21/00
Inventor 赵志超马朋高李晓艳胡育林龚光碧梁滔郑聚成王永峰贾慧青李波陈建刚秦传高邵卫肖晔翟云芳
Owner PETROCHINA CO LTD
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