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Preparation method of nano-silica having liquid rubber-grafted surface

A technology of nano-silica and liquid rubber, which is applied in the field of rubber fillers, can solve the problems of restricting large-scale production, unfavorable product industrialization, and difficulty in large-scale preparation, so as to shorten the vulcanization time, improve processing technology, and compatibility. Improved effect

Inactive Publication Date: 2019-11-15
安徽工程大学宣城产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These modified fillers can improve the performance of polymers to a certain extent, but they are difficult to prepare in large quantities, which also limits their large-scale production and is not conducive to the industrialization of products.

Method used

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  • Preparation method of nano-silica having liquid rubber-grafted surface
  • Preparation method of nano-silica having liquid rubber-grafted surface
  • Preparation method of nano-silica having liquid rubber-grafted surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 150g of fumed silica (nano silica, particle size 25nm), 45g of liquid natural rubber, 4.5g of maleic anhydride, 2.25g of azobisisobutyronitrile, and 500ml of 1,4-dioxane into the reaction In the kettle, the product was obtained by mechanical stirring for 24 hours at a reaction temperature of 60°C.

[0022] The obtained product was suction filtered and then dissolved by adding 1000ml of dichloromethane to wash away the unreacted liquid natural rubber. The operation was repeated four times and placed in a vacuum drying oven at 70℃ for 30h to obtain the final grafted product. -Nano silica with liquid rubber grafted on the surface. The thermal weight loss analysis shows that the grafting rate is 5.4%, that is, the grafted liquid rubber accounts for 5.4% of the weight of the fumed silica (nano silica).

[0023] The vulcanization and mechanical properties of silica before and after grafting were compared. The silica before and after grafting was dried under conditions: 70℃×...

Embodiment 2

[0029] Weigh 200g of white carbon black (particle size 7nm), 60g of liquid natural rubber, 9g of maleic anhydride, 4.5g of azobisisobutyronitrile, and 1500ml of 1,4-dioxane into the reactor. The reaction temperature is The product was obtained by mechanical stirring for 48 hours at 65°C.

[0030] The obtained product was suction filtered and 1000ml of dichloromethane was added to wash off the unreacted liquid natural rubber. The operation was repeated four times and dried in a vacuum drying oven at 70° C. for 30 hours to obtain the final product. The thermal weight loss analysis shows that the liquid rubber accounts for 7.2% of the silica weight.

[0031] Vulcanization and mechanical performance test

[0032] The vulcanization and mechanical properties of silica before and after grafting were compared. The silica before and after grafting was dried under conditions: 70℃×5h. For mixing on an open mill, first plasticize the raw rubber, add stearic acid and ZnO to tap the rubber after...

Embodiment 3

[0038] Add white carbon black (particle size 12nm) 8g, liquid butadiene rubber (molecular weight 3k) 5.6g, maleic anhydride 0.56g, azobisisobutyronitrile 0.28g, and tetrahydrofuran 50ml, and put them into a pressure flask, at the reaction temperature The product was obtained by mechanical stirring for 48h at 65°C.

[0039] The obtained product was dissolved by adding 10 ml of dichloromethane to wash away the unreacted liquid butadiene rubber, and the operation was repeated four times and placed in a vacuum drying oven at 80° C. to obtain the final product. Liquid butadiene rubber accounts for 6.72% of the weight of the silica.

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Abstract

The invention relates to a preparation method of nano-silica having a liquid rubber-grafted surface. The preparation method comprises the following steps: dispersing nano-silica in a solvent, then adding a double bond-containing coupling agent, a radical initiator and liquid rubber, performing a reaction at a certain temperature for a certain period of time, and washing and drying the obtained reaction product after the reaction is finished in order to obtain the nano-silica having the liquid rubber-grafted surface. The preparation method adopting a one-pot process has the advantages of simplicity in operation, mild reaction conditions and convenience in large-scale production; and the compatibility between the nano-silica having the liquid rubber-grafted surface and a rubber-plastic matrix material is effectively improved, and a good foundation is laid for the effective exertion of synergistic performances of different components in the formula of the rubber-plastic material.

Description

Technical field [0001] The invention belongs to the technical field of rubber fillers, and specifically relates to a preparation method of nano-silica grafted with liquid rubber on the surface. Background technique [0002] Nano silica (SiO 2 , White carbon black) is a common inorganic material, often used to reinforce filled rubber and plastics. Nano SiO 2 It can improve the mechanical properties of rubber and plastic materials to a certain extent. But unmodified nano SiO 2 The surface contains silanols with strong polarity and has a large specific surface area, which is very easy to form aggregates in the matrix material. This is not good for nano SiO 2 The dispersion in the matrix rubber and plastic materials affects the microstructure and performance of nanocomposites. Therefore, to prepare nanocomposite materials with ideal comprehensive performance, it is necessary to 2 Make proper surface modification. [0003] There are many ways to chemically modify silica. Usually, org...

Claims

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Application Information

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IPC IPC(8): C08K9/08C08K3/36
CPCC08K3/36C08K9/08C08K2201/003C08K2201/011
Inventor 相益信沈显荣宋庆平查冬旺赵海兵耿雅婷胡庆松
Owner 安徽工程大学宣城产业技术研究院有限公司