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Preparation method of silicon dioxide/graphene modified rubber composite material

A graphene modification, silica technology, applied in the direction of rolling resistance optimization, transportation and packaging, special tires, etc., can solve the problem of antistatic, no significant improvement in thermal conductivity, inability to improve various properties of rubber, self-polymerization compounds Expensive and other problems, to achieve the effect of increasing mechanical properties, avoiding water pollution problems, and reducing mixing energy consumption

Active Publication Date: 2022-07-08
HENAN UNIVERSITY
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  • Claims
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Problems solved by technology

[0004] In recent years, a variety of patented technologies involving the preparation of natural rubber nanocomposites from graphene have been disclosed, which can be roughly classified into two categories: one is a single filler-reinforced rubber: (1) non-covalent bond modification method: in a certain Under the action of temperature and mechanical stirring, self-polymerizing monomers such as dopamine are used to form a polymer coating layer on the surface of graphene to modify nanomaterials, and then dry-mixed to prepare composite materials, but self-polymerizing compounds are expensive , which is not conducive to industrial production; (2) covalent bond modification method: first prepare nanomaterial emulsion, introduce silane coupling agent into the emulsion, thereby regulating its surface activity to improve the dispersion in composite materials, and improve the comprehensive performance of composite materials , but the silane coupling agent is introduced as a filler, which cannot improve the properties of rubber, and there are certain problems in the application of special fields (such as silicon dioxide, which can only improve the mechanical properties of rubber, and it can only improve the antistatic and thermal conductivity of rubber. No significant improvement effect); the other type is two or more types of filler-reinforced rubber: first functionalize each single filler, and then use the electrostatic adsorption or chemical reaction of the modified filler surface functional groups to prepare a hybrid Multi-component particles use the synergistic reinforcing effect of hybrid particles to improve the comprehensive performance of rubber composites. However, binary particles prepared only by electrostatic adsorption will separate during dry mixing. cannot fully interact with each other, making it difficult to achieve synergistic reinforcement

Method used

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  • Preparation method of silicon dioxide/graphene modified rubber composite material
  • Preparation method of silicon dioxide/graphene modified rubber composite material
  • Preparation method of silicon dioxide/graphene modified rubber composite material

Examples

Experimental program
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Effect test

Embodiment 1

[0041] with graphene dry powder (see figure 1 The content of (a) is 100 phr, take graphene dry powder, 5 phr ethanol, 2 phr polyvinylpyrrolidone, add 3900 phr distilled water, ultrasonically stir for 3 h, perform suction filtration, wash multiple times, and dry to obtain surface-modified polyvinylpyrrolidone. Functionalized graphene, i.e. powdered hydrophilic graphene;

[0042] Based on the functionalized graphene dry powder content of 12 phr, take 1278 phr sodium silicate (n=3.2) and 1566 phr distilled water, heat up to 68 ° C, and stir for 20 min to obtain a graphene-sodium silicate aqueous solution; stir at a rotating speed of 600 rad / min , slowly add dilute sulfuric acid solution (wt = 20%) dropwise to the graphene-sodium silicate aqueous solution until the pH of the solution = 8-9, then heat up to 80 ° C for 3 h, and then slowly add 72phr modifier ( γ-glycidyl ether oxypropyltrimethoxysilane: ethanol=1:1), after the modifier is completely added, the constant temperature ...

Embodiment 2

[0047] Based on the graphene dry powder content of 100 phr, take graphene dry powder, 5 phr ethanol, and 2 phr polyvinylpyrrolidone, add them to 3900 phr distilled water, ultrasonically stir for 3 hours, suction filter, wash multiple times, and dry to obtain the surface modified with polyvinylpyrrolidone. Graphene, namely powdered hydrophilic graphene;

[0048] Based on the functionalized graphene dry powder content of 12 phr, and taking 639 phr of sodium silicate (n=3.2) and 783 phr of distilled water, the temperature was raised to 70 ° C, and after stirring for 20 min, the graphene-sodium silicate aqueous solution was obtained; under the rotating speed of 600 rad / min Stir, slowly add dilute sulfuric acid solution (wt = 20%) to the graphene-sodium silicate aqueous solution until the pH of the solution = 8-10, then heat up to 80 ° C for 3 hours, and then slowly add 36phr modifier to the reaction system (γ-glycidyl ether oxypropyltrimethoxysilane: ethanol=1:1), after the modifi...

Embodiment 3

[0052] Based on the graphene dry powder content of 100 phr, take 5 phr of ethanol and 2 phr of polyvinyl pyrrolidone, add them into 3900 phr of distilled water, and after ultrasonic stirring for 3 hours, suction filtration, multiple washings, and drying to obtain the surface-modified functionalized graphene with polyvinyl pyrrolidone, That is, powdered hydrophilic graphene;

[0053] Based on the content of functionalized graphene dry powder of 12 phr, take 319.5 phr sodium silicate (n=3.2) and 391.5 phr distilled water, heat up to 69 ° C, and stir for 20 min to obtain a graphene-sodium silicate aqueous solution; at a rotating speed of 600 rad / min Under stirring, dilute sulfuric acid solution (wt = 20%) was slowly added dropwise to the graphene-sodium silicate aqueous solution until the pH of the solution = 8-10, then the temperature was raised to 80 °C for 3 h, and then 18phr was slowly added to the reaction system for modification agent (γ-glycidyl ether oxypropyltrimethoxysi...

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Abstract

The preparation method of the silicon dioxide / graphene modified rubber composite material comprises the following steps: dispersing graphene in a solvent to obtain a graphene dispersion liquid, and adding an amphiphilic polymer into the graphene dispersion liquid to react to obtain a hydrophilic graphene dispersion liquid; carrying out spray drying to obtain powdery hydrophilic graphene of which the surface is modified with an amphiphilic polymer; the preparation method comprises the following steps: dispersing powdery hydrophilic graphene in a silicon source compound aqueous solution to obtain a graphene-silicon source compound solution, and adjusting the pH value of the graphene-silicon source compound solution until a silicon source compound is hydrolyzed to obtain a mixed filter cake of silicon dioxide graphene-based binary particles; diluting the mixed filter cake into an emulsion as a filler, adding the emulsion into latex to obtain a mixed system, adding a flocculant into the mixed system to induce demulsification of the latex to obtain flocculate, and adding a processing aid into the flocculate to obtain the silicon dioxide / graphene modified rubber composite material. The mechanical property, wear resistance and thermal conductivity of the rubber composite material are improved.

Description

technical field [0001] The invention relates to the field of tread rubber composite materials, in particular to a preparation method of a silica / graphene modified rubber composite material. Background technique [0002] As one of the main components of aviation tires, tread rubber needs to withstand high speed and high load, and can evenly transfer static charge to the ground when the aircraft takes off and land. In addition, it needs to release the heat generated during the taxiing process in time. , the use conditions are very harsh. This requires that when designing aircraft tire treads, not only many factors to be considered for ordinary tire treads, such as wear resistance, wet skid resistance, etc., but also for its special working environment, many complex factors must be considered. Factors design tread compounds with more demanding performance requirements. [0003] Graphene has similar reinforcing properties to silica and can be used as a reinforcing filler for r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L7/00C08L9/06C08L21/00C08K9/12C08K9/04C08K9/06C08K3/04C08K3/36C08C1/16B60C1/00
CPCC08L7/00C08L9/06C08L21/00C08C1/14B60C1/0016C08L2201/04C08K9/12C08K9/08C08K9/06C08K3/042C08K3/36Y02T10/86
Inventor 丁涛吕晓慧李小红张治军房晓敏徐元清张立群
Owner HENAN UNIVERSITY
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