CN115433391A - Carbon material-loaded silicon dioxide hybrid filler and preparation method and application thereof - Google Patents

Carbon material-loaded silicon dioxide hybrid filler and preparation method and application thereof Download PDF

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CN115433391A
CN115433391A CN202211134489.2A CN202211134489A CN115433391A CN 115433391 A CN115433391 A CN 115433391A CN 202211134489 A CN202211134489 A CN 202211134489A CN 115433391 A CN115433391 A CN 115433391A
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carbon material
silicon dioxide
hybrid filler
silica
physically modified
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李崇兵
徐旗
汪燕
连伟平
吕伟
李琳
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Qingdao University of Science and Technology
Prinx Chengshan Shandong Tire Co Ltd
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Qingdao University of Science and Technology
Prinx Chengshan Shandong Tire Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B60—VEHICLES IN GENERAL
    • B60C—VEHICLE TYRES; TYRE INFLATION; TYRE CHANGING; CONNECTING VALVES TO INFLATABLE ELASTIC BODIES IN GENERAL; DEVICES OR ARRANGEMENTS RELATED TO TYRES
    • B60C1/00—Tyres characterised by the chemical composition or the physical arrangement or mixture of the composition
    • B60C1/0016—Compositions of the tread
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica

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  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a carbon material-loaded silicon dioxide hybrid filler and a preparation method and application thereof, belonging to the field of new materials. The carbon material-supported silica hybrid filler is formed by self-assembling a plant polyphenol physically-modified carbon material and alkene compound physically-modified silica through physical effects such as hydrogen bonds. The carbon material-loaded silicon dioxide hybrid filler has excellent functions of electric conduction, heat conduction and the like, solves the insulativity of a silicon dioxide filled rubber plastic product, and can solve the application problems of high energy consumption, high pollution, unstable performance and the like of silane coupling agent modified silicon dioxide by adopting alkene compounds to physically modify the silicon dioxide. The preparation process is simple, low in cost and less in pollution, and can be uniformly dispersed in a polymer matrix, so that the mechanical property, the electrical property and the thermal property of the polymer-based nano composite material are obviously improved.

Description

Carbon material-loaded silicon dioxide hybrid filler and preparation method and application thereof
Technical Field
The invention relates to the field of new materials, in particular to a carbon material-loaded silicon dioxide hybrid filler and a preparation method and application thereof.
Background
Polymeric materials, particularly rubber materials, are often reinforced to be of practical value. At present, the most commonly used reinforcing materials are carbon black and white carbon black (silicon dioxide), the white carbon black has hydroxyl on the surface, has higher surface energy and hydrophilic surface, is not good in compatibility with most polymer materials, is difficult to infiltrate and disperse in most polymer materials, so that the reinforcing performance is reduced, the compatibility of the white carbon black and a polymer matrix can be improved only by means of a silane coupling agent, but the reinforcing effect of the white carbon black subjected to silanization modification is far inferior to that of the carbon black.
The white carbon black is an ideal filler for green tires, and can reduce the heat generation, the lag and the rolling resistance of the tires, thereby saving fuel and prolonging the service life of the tires; and the wet skid resistance and the wear resistance of the tire can be improved, so that the problem of magic triangles of the tire is effectively solved. However, white carbon black is a strong polar filler, and common tire rubber materials (natural rubber, butadiene rubber and styrene butadiene rubber) are nonpolar materials, and due to the large difference in polarity between the two materials, the unmodified white carbon black has the following problems in the preparation process of the tire rubber material: (1) the white carbon black has poor dispersibility in the rubber matrix, is easy to agglomerate and is difficult to eat; (2) the compatibility between the rubber matrix and the white carbon black interface is poor, and the mechanical property of the sizing material is poor; (3) the heat generation in the mixing process is large, so that scorching and the molecular weight reduction of rubber are easily caused; (4) the accelerator and the anti-aging agent are easy to adsorb, and the vulcanization speed and the aging performance are reduced. Therefore, white carbon black must be modified when it is used for the production of tires.
The silane coupling agent method is the most commonly used white carbon black surface modification method. The silane coupling agents used are, for example, si-69, si-75, KH590 and the like. However, since the silane coupling agent undergoes severe self-condensation, the reactivity is low, and thus the efficiency of modifying the carbon black is low. The carbon material is a nano material integrating excellent mechanical, electric and heat conduction properties and the like, and mainly comprises four types, namely carbon nano tubes, graphene, carbon nano fibers and nano carbon spheres. The carbon material is added into the polymer matrix, so that the mechanical property of the polymer can be effectively improved, and the composite material can be endowed with excellent multiple functions of electric conduction, heat conduction, electromagnetic shielding, gas barrier and the like. Although research on polymer/carbon material nanocomposites has achieved extraordinary performance, there are still many challenges to its commercialization.
In view of the importance of the white carbon black in the tire industry, the defects of the existing method for modifying the white carbon black by using the silane coupling agent, the limitation of the application performance of single filler and the like, the invention adopts the hybrid filler formed by reasonably combining and matching the fillers.
Disclosure of Invention
In view of the above situation, the invention aims to develop a carbon material-supported silica hybrid filler with good electrical and thermal conductivity, low cost, simple preparation process and environmental protection, and the carbon material-supported silica hybrid filler is used for preparing a high-performance polymer-based nanocomposite material.
The basic principle of the invention is as follows: firstly, preparing a carbon material physically modified by plant polyphenol through the auxiliary dispersion of the plant polyphenol. On one hand, the carbon material and the plant polyphenol are adsorbed together through pi-pi conjugated stacking effect, so that the structure and the performance of the carbon material are well protected; on the other hand, plant polyphenols impart a large number of phenolic hydroxyl groups to the surface of the carbon material. Then, the silica is physically modified with an alkene compound, and a group capable of producing physical adsorption such as a hydrogen bond with a phenolic hydroxyl group is modified on the surface of the silica. And finally, the preparation of the carbon material-loaded silica hybrid filler is realized by utilizing the physical actions such as hydrogen bonds between the carbon material physically modified by the plant polyphenol and the silica physically modified by the vinyl compound. The carbon material-supported silica hybrid filler is applied to the preparation of a high-performance polymer-based nano composite material, and through the hybridization of the carbon material and the silica, the carbon material-supported silica hybrid filler can inhibit respective agglomeration and exert a synergistic dispersion effect, and the silica can play a role of volume exclusion to remarkably reduce the percolation threshold of the carbon material, so that the cost of the polymer/carbon material nano composite material is reduced.
The specific technical scheme of the invention is as follows:
a preparation method of a carbon material-loaded silica hybrid filler comprises the following steps: mixing water dispersion of plant polyphenol physically modified carbon material and dispersion of vinyl compound physically modified silica by means of ultrasound or stirring, so that the vinyl compound physically modified silica is adsorbed to the surface of the plant polyphenol physically modified carbon material through physical actions such as hydrogen bonds and the like, and obtaining the carbon material-loaded silica hybrid filler, wherein the mass ratio of the carbon material to the silica is 1:1 to 1:150, preferably 1.
The preparation method of the plant polyphenol physically modified carbon material comprises the following steps: preparing a plant polyphenol physically-modified carbon material by using a carbon material as a raw material, using plant polyphenol as a dispersing auxiliary agent, using water as a dispersing medium and adopting ultrasound or high-speed shearing of the carbon material; the plant polyphenol comprises one or more of hydrolyzed tannin, condensed tannin or complex polyphenol, or a natural product taking the plant polyphenol as a main component, and the mass fraction is 0.005wt% -50wt%; the carbon material comprises 0.5-5% of graphene, multi-walled carbon nanotubes, carbon fibers, mesocarbon microbeads, natural graphite, glassy carbon, hard carbon, porous activated carbon, highly oriented graphite, carbon black, diamond and fullerene by mass.
The hydrolyzed tannin used in the invention is preferably tannic acid, tara tannin, yellow gallol, dehydro-digallic acid, valoneac acid, geraniin, glucose gallate or propyl gallate.
The condensed tannin used in the present invention is preferably procyanidin, cercis negundo tannin, larch bark tannin, myrica bark tannin, tea tannin, red pink tannin, epigallocatechin gallate, epicatechin, gallocatechin gallate or epicatechin gallate.
The complex polyphenol used in the invention is a polyphenol compound with the structural characteristics of both hydrolyzed tannin and condensed tannin in the molecular structure, and preferably quercus acutissima tannin or quercitrin.
The natural product with plant polyphenol as main component is valonia extract, larch bark extract, areca extract, chestnut extract, quebracho extract or red root extract.
The preparation method of the physically modified silicon dioxide by the alkene compound comprises the following steps: adopting silicon dioxide as a raw material, an alkene compound as a modifier, and water or alcohol or a mixed solvent of the water and the alcohol as a dispersion medium, and stirring for reaction to obtain alkene compound physically modified silicon dioxide; the mass fraction of the silicon dioxide is 1wt% -50wt%; the alkene compound is as follows: one or more of enol (such as oleyl alcohol, etc.), enamine (such as oleyl amine, etc.), olefine acid (such as oleic acid, linoleic acid, eleostearic acid, etc.), oleamide and alkene compounds containing phenolic hydroxyl (such as urushiol, etc.) in the solvent, wherein the mass fraction of the mixture is 0.01-10 wt%.
The carbon material-loaded silica hybrid filler can be dispersed in a polymer matrix (such as rubber) by a solution blending, emulsion blending or melt blending method to prepare a polymer-based nanocomposite material with the characteristics of low cost, high performance, multiple functions and the like.
The carbon material-loaded silicon dioxide hybrid filler disclosed by the invention contains plant polyphenol which is an important component, and the structure of the plant polyphenol contains a large number of active chemical reaction sites such as phenolic hydroxyl, ortho-hydrogen and the like, so that the hybrid filler can be endowed with good solvent dispersibility to facilitate liquid phase processing, and the function of an interface regulator can be exerted to improve the interface adhesion of a composite material.
The invention has the beneficial effects that: (1) Compared with the traditional silane coupling agent modified white carbon black, the olefin modified white carbon black has better dispersibility and reinforcing effect in non-polar rubber, so that the rubber material prepared based on the olefin modified white carbon black has higher strength and wet-skid resistance, lower abrasion and dynamic compression heat generation; (2) The conductive carbon material is hybridized with the reinforcing material silicon dioxide, so that the synergistic effect of ' 1+1> ' 2 ' can be exerted, and the dosage of expensive filler can be reduced through the collocation of the cheap filler and the expensive filler, so that the cost is effectively reduced; (3) Unsaturated double bonds capable of participating in rubber vulcanization are introduced to the surface of the white carbon black, so that the interface strength of the white carbon black and the rubber matrix can be further improved, and the mechanical property of the rubber material is further improved.
Drawings
Fig. 1 is a scanning electron micrograph of the graphene-supported silica filler prepared in example 1 at different magnifications.
FIG. 2 is a scanning electron micrograph of the natural rubber nanocomposite prepared in example 1 at different magnifications.
FIG. 3 is a scanning electron micrograph of the multi-walled carbon nanotube-loaded silica filler prepared in example 2 at different magnifications.
FIG. 4 is a scanning electron micrograph of the natural rubber nanocomposite prepared in example 2 at different magnifications.
Detailed Description
The invention is explained in further detail below by means of specific embodiments with reference to the drawings. It is to be understood that the following examples are intended to illustrate the invention and are not intended to limit its scope.
Example 1
Adding 1g of graphene and 0.01g of tannic acid into 100ml of water, wherein the mass fractions of the graphene and the tannic acid in the water are 1wt% and 0.01wt%, respectively, and performing ultrasonic treatment under the ultrasonic condition of 100W of ultrasonic power and 1h of ultrasonic time to obtain the aqueous dispersion of the tannic acid physically modified graphene. 1g of oleylamine and 50g of silicon dioxide are added to 100ml of ethanol, the mass fractions of the oleylamine and the silicon dioxide in the ethanol are 1wt% and 33wt%, respectively, and the mixture is stirred at room temperature for 2 hours. And then, stirring and mixing the aqueous dispersion of the tannic acid physically modified graphene and the dispersion of the oleylamine modified silica for 1 hour to obtain the graphene-supported silica hybrid filler dispersion. And finally, filtering and drying to obtain the graphene-loaded silicon dioxide hybrid filler, wherein the mass ratio of the graphene to the silicon dioxide is 1:50. fig. 1 is a scanning electron microscope picture of a graphene-supported silica hybrid filler. As can be seen from the figures, the silicon dioxide is uniformly supported on the carbon material, which indicates that the combination of the two is strong.
The prepared graphene-loaded silica hybrid filler is applied to the tread rubber formula in the table 1 to prepare the natural rubber nanocomposite. The natural rubber nanocomposite has a tensile strength of 29.7MPa, an elongation at break of 641.1%, a tear strength of 105.46kN/m, a tan 60 ℃ of 0.0870, and an electrical conductivity of 1.003 x 10 -6 S/m, thermal conductivity of 0.2563 W.m -1 ·K -1 . Fig. 2 is a scanning electron micrograph of the graphene-loaded silica hybrid filler natural rubber nanocomposite, in which the fillers are uniformly distributed and do not have an obvious agglomeration phenomenon, which shows that the dispersibility of the graphene-loaded silica hybrid filler is improved.
Table 1 composite material formulation table
Figure BDA0003851131260000041
Example 2
Adding 1g of multi-walled carbon nanotube and 0.01g of tannic acid into 100ml of water, wherein the mass fractions of the multi-walled carbon nanotube and the tannic acid in the water are 1wt% and 0.01wt%, respectively, and performing ultrasonic treatment under the ultrasonic condition that the ultrasonic power is 100W and the ultrasonic time is 1h to obtain the aqueous dispersion of the tannic acid physically modified multi-walled carbon nanotube. 1g of oleylamine and 50g of silicon dioxide are added to 100ml of ethanol, the mass fractions of the oleylamine and the silicon dioxide in the ethanol are 1wt% and 33wt%, respectively, and the mixture is stirred at room temperature for 2 hours. And then stirring and mixing the aqueous dispersion of the multi-walled carbon nano-tubes physically modified by tannic acid and the dispersion of the silicon dioxide modified by oleylamine for 1h to obtain the multi-walled carbon nano-tube loaded silicon dioxide hybrid filler dispersion. And finally, filtering and drying to obtain the multiwalled carbon nanotube-loaded silicon dioxide hybrid filler, wherein the mass ratio of the multiwalled carbon nanotube to the silicon dioxide is 1:50. FIG. 3 is a scanning electron microscope image of a multiwalled carbon nanotube loaded silica hybrid filler. As can be seen from the pictures, the silicon dioxide is uniformly loaded on the multi-wall carbon nano-tube, which shows that the combination of the two is strong.
The prepared multi-walled carbon nanotube-loaded silica hybrid filler is applied to a tread rubber formula according to a formula table of table 1 to prepare the natural rubber nanocomposite. The natural rubber nanocomposite has a tensile strength of 30.2MPa, an elongation at break of 671.8%, a tear strength of 122.5kN/m, a tan of 0.087 at 60 ℃, and an electrical conductivity of 4.111 x 10 -4 S/m, thermal conductivity of 0.2615 W.m -1 ·K -1 The hybrid filler can obviously improve the tensile strength, elongation at break, tear strength, electrical conductivity and thermal conductivity of the composite material, and reduce the dynamic heat generation of the composite material more effectively. FIG. 4 is a scanning electron micrograph of the multi-walled carbon nanotube-loaded silica hybrid filler natural rubber nanocomposite, wherein the filler is uniformly distributed without obvious agglomeration, which shows that the dispersibility of the multi-walled carbon nanotube-loaded silica hybrid filler is improved.
Example 3
Adding 1g of multi-walled carbon nanotube and 0.01g of yellow gallol into 100ml of water, wherein the mass fractions of the two in the water are 1wt% and 0.01wt%, respectively, and performing ultrasonic treatment under the ultrasonic condition of 100W of ultrasonic power and 1h of ultrasonic time to obtain the aqueous dispersion of the yellow gallol physically modified multi-walled carbon nanotube. 1g of oleyl alcohol and 50g of silicon dioxide were added to 100ml of ethanol at mass fractions of 1wt% and 33wt% in ethanol, respectively, and stirred at room temperature for 2 hours. And then, stirring and mixing the aqueous dispersion of the multiwall carbon nanotube physically modified by the yellow gallool and the dispersion of the oleyl alcohol modified silica for 1 hour to obtain the multiwall carbon nanotube-loaded silica hybrid filler dispersion. And finally, filtering and drying to obtain the multiwalled carbon nanotube-loaded silicon dioxide hybrid filler, wherein the mass ratio of the multiwalled carbon nanotube to the silicon dioxide is 1:50.
the prepared multi-walled carbon nanotube-loaded silica hybrid filler is applied to a tread rubber formula according to a formula table of table 1 to prepare the natural rubber nanocomposite. The natural rubber nanocomposite has a tensile strength of 29.2MPa, an elongation at break of 651.6%, a tear strength of 115.4kN/m, a tan of 0.093 at 60 ℃ and an electrical conductivity of 6.278 × 10 -5 S/mThe thermal conductivity is 0.2432 W.m -1 ·K -1 The hybrid filler can obviously improve the tensile strength, elongation at break, tear strength, electrical conductivity and thermal conductivity of the composite material, and can reduce the dynamic heat generation of the composite material more effectively.
Example 4
Adding 1g of multi-walled carbon nanotube and 0.1g of tannic acid into 100ml of water, wherein the mass fractions of the two in the water are 1wt% and 0.01wt%, respectively, and performing ultrasonic treatment under the ultrasonic condition of 100W of ultrasonic power and 1h of ultrasonic time to obtain an aqueous dispersion of tannic acid physically modified multi-walled carbon nanotube. 5g oleylamine and 50g of silica were added to 100ml of ethanol and stirred at room temperature for 2h. And then stirring and mixing the aqueous dispersion of the multi-walled carbon nano-tubes physically modified by tannic acid and the dispersion of the silicon dioxide modified by oleylamine for 1h to obtain the multi-walled carbon nano-tube loaded silicon dioxide hybrid filler dispersion. And finally, filtering and drying to obtain the multi-walled carbon nanotube-loaded silica hybrid filler, wherein the mass ratio of the multi-walled carbon nanotube to the silica is 1:20. the prepared multi-walled carbon nanotube-loaded silica hybrid filler is applied to a tread rubber formula according to a formula table of table 1 to prepare the natural rubber nanocomposite. The natural rubber nanocomposite had a tensile strength of 29.2MPa, an elongation at break of 643.7%, a tear strength of 109.3kN/m, a tan 60 ℃ of 0.103, and an electrical conductivity of 6.86 x 10 -5 S/m, thermal conductivity of 0.2347 W.m -1 ·K -1 The hybrid filler can obviously improve the tensile strength, elongation at break, tear strength, electrical conductivity and thermal conductivity of the composite material, and can reduce the dynamic heat generation of the composite material more effectively.
Comparative example 1
1g of oleylamine and 50g of silicon dioxide are added to 100ml of ethanol, the mass fractions of the oleylamine and the silicon dioxide in the ethanol are 1wt% and 33wt%, respectively, and the mixture is stirred at room temperature for 2 hours. And then filtering and drying to obtain the oleylamine modified silica filler.
The prepared oleylamine modified silica filler was applied to a tread rubber formulation according to the formulation table of table 1 to prepare a natural rubber nanocomposite. The natural rubber nano composite material has the tensile strength of 26.4MPa, the elongation at break of 589.8 percent and tearing strengthA crack strength of 86.7kN/m, tan 60 ℃ of 0.085, and an electrical conductivity of 6.56 x 10 -9 S/m, thermal conductivity of 0.185 W.m -1 ·K -1 。
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the scope of the present invention is not limited thereto. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (5)

1. The carbon material-loaded silica hybrid filler is characterized by consisting of a carbon material physically modified by plant polyphenol and silica physically modified by an alkene compound, wherein the mass ratio of the carbon material to the silica is 1:1 to 1:150.
2. a method for preparing the carbon material-supported silica hybrid filler of claim 1: the method is characterized in that water dispersion of plant polyphenol physically modified carbon material and dispersion of alkene compound physically modified silica are mixed in an ultrasonic or stirring mode, so that the alkene compound physically modified silica is adsorbed to the surface of the plant polyphenol physically modified carbon material through physical action, and the carbon material-loaded silica hybrid filler is obtained.
3. The method for preparing the carbon material-supported silica hybrid filler according to claim 2, wherein the method for preparing the plant polyphenol physically modified carbon material comprises the following steps: graphite and/or derivatives thereof are used as raw materials, plant polyphenol is used as a dispersing aid, water is used as a dispersing medium, the carbon material is subjected to ultrasonic or high-speed shearing to prepare the plant polyphenol physically-modified carbon material, the content of the plant polyphenol in a dispersing solution is 0.005-50 wt%, and the content of the carbon material in the dispersing solution is 0.5-5 wt%.
4. The preparation method of the carbon material-supported silica hybrid filler according to claim 2 or 3, characterized in that the preparation method of the vinyl compound physically modified silica is: adopting silicon dioxide as a raw material, an alkene compound as a modifier, and water or alcohol or a mixed solvent of the water and the alcohol as a dispersion medium, and stirring for reaction to obtain silicon dioxide physically modified by the alkene compound; the content of the silicon dioxide in the solvent is 1wt% -50wt%; the alkene compound is one or a mixture of more of enol, enamine, olefine acid, oleic acid amide and alkene compounds containing phenolic hydroxyl, and the content of the alkene compounds in the solvent is 0.01wt% -10wt%.
5. The use of the carbon material-supported silica hybrid filler of claim 1, wherein the hybrid filler can be dispersed in a polymer matrix by solution blending, emulsion blending or melt blending to produce a high performance polymer-based nanocomposite.
CN202211134489.2A 2022-09-19 2022-09-19 Carbon material-loaded silicon dioxide hybrid filler and preparation method and application thereof Pending CN115433391A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030199626A1 (en) * 2002-04-17 2003-10-23 Chen-Chy Lin Addition of polar polymer to improve tear strength and processing of silica filled rubber
JP6097875B1 (en) * 2016-01-07 2017-03-15 深▲セン▼先進技術研究院 Silica filler, silica filler surface treatment method and epoxy resin composite
CN107236150A (en) * 2017-07-07 2017-10-10 青岛科技大学 A kind of novel graphite alkene nonloaded silica hydridization filler and preparation method thereof, application
CN113789066A (en) * 2021-08-18 2021-12-14 浦林成山（青岛）工业研究设计有限公司 Olefin modified white carbon black for rubber and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030199626A1 (en) * 2002-04-17 2003-10-23 Chen-Chy Lin Addition of polar polymer to improve tear strength and processing of silica filled rubber
JP6097875B1 (en) * 2016-01-07 2017-03-15 深▲セン▼先進技術研究院 Silica filler, silica filler surface treatment method and epoxy resin composite
CN107236150A (en) * 2017-07-07 2017-10-10 青岛科技大学 A kind of novel graphite alkene nonloaded silica hydridization filler and preparation method thereof, application
CN113789066A (en) * 2021-08-18 2021-12-14 浦林成山（青岛）工业研究设计有限公司 Olefin modified white carbon black for rubber and preparation method thereof

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Application publication date: 20221206