CN112358693A - Interface modified chlorinated polyethylene rubber based on novel reinforcing agent and preparation method thereof - Google Patents
Interface modified chlorinated polyethylene rubber based on novel reinforcing agent and preparation method thereof Download PDFInfo
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- CN112358693A CN112358693A CN202011271783.9A CN202011271783A CN112358693A CN 112358693 A CN112358693 A CN 112358693A CN 202011271783 A CN202011271783 A CN 202011271783A CN 112358693 A CN112358693 A CN 112358693A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/26—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L23/28—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
- C08L23/286—Chlorinated polyethylene
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
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Abstract
The invention discloses an interface modified chlorinated polyethylene rubber based on a novel reinforcing agent and a preparation method thereof, wherein the interface modified chlorinated polyethylene rubber comprises the following raw materials in parts by weight: 80 parts of chlorinated polyethylene, 10 parts of reinforcing agent, 5 parts of coupling agent, 25 parts of flame retardant, 10 parts of stabilizer, 2 parts of auxiliary stabilizer, 1.5 parts of lubricant, 6 parts of halogen-free plasticizer, 3 parts of vulcanizing agent and 2 parts of vulcanizing assistant; the reinforcing agent is a nano filler, the nano filler is a boron carbide nanowire, and the boron carbide nanowire is obtained by heating a mixture of a carbon nanotube and boron powder by using the carbon nanotube as a template; the coupling agent is graphene, and the graphene is a high-quality graphene sheet and is directly prepared from graphite; the stabilizer is a combination of magnesium oxide, zinc glycerolate as a stabilizer and magnesium stearate as a stabilizer. The base material, the coupling agent, the reinforcing agent and the stabilizing agent are safe and environment-friendly, do not contain substances which are harmful to the environment greatly, and follow the development trend of green chemistry.
Description
Technical Field
The invention relates to the technical field of rubber, in particular to an interface modified chlorinated polyethylene rubber based on a novel reinforcing agent and a preparation method thereof.
Background
The rubber reinforcing agent is a compounding agent capable of improving the strength of rubber products. Reinforcing materials for the rubber industry have been based on carbon black, which accounts for about 60% or more of the total rubber filler. There are a number of negative effects in the preparation and application of carbon black as a reinforcing material. Carbon black is a by-product of the petroleum industry, and is costly and highly polluting during use, and therefore, alternatives to carbon black are being sought.
For this reason, many researchers have developed many new reinforcing fillers, most of which are inorganic reinforcing fillers, mainly silicates and calcium carbonate mineral powders. If the powder is used for obtaining good application effect in a rubber system, a common problem to be solved is surface modification. After the surface modification treatment, the non-metallic mineral can eliminate the surface high energy potential, adjust the hydrophobicity, improve the compatibility and the interface bonding force with the organic base material, enhance the mechanical strength of the material and improve the comprehensive performance of the material, thereby meeting the requirements of modern new materials and new technologies.
Nanofillers are ideal reinforcing materials and can achieve a combination of strength and toughness, but in practice the effect is much lower than predicted theoretically, mainly due to interface problems between the filler and the matrix. Many approaches have been explored to improve the dispersion of nanofillers and the filler-matrix interface, including surface treatments such as silane coupling agents and grafting onto polymer chains, to some extent reducing the interface problems. Therefore, there is an urgent need to find a novel interfacial modifier which can simultaneously achieve uniform dispersion of the nano-filler and improve the interfacial bonding effect in the nanocomposite.
Graphene has been a research hotspot due to its special high crystallinity and mechanical strength, and in polymer matrix composites, graphene with a high specific surface area can be an excellent interface modifier through pi-pi interaction, hydrogen bonding, van der waals force, electrostatic interaction, chemical adhesion, and the like.
In view of the above, a graphene interface engineering technology is utilized to bond a boron carbide nanowire and graphene together to obtain a graphene-coated boron carbide nanowire so as to enhance the dispersibility of the nanowire in a matrix, thereby significantly improving the strength and toughness of a rubber composite material, which has become a new way for developing a tough nanocomposite material, however, how to apply the graphene-coated boron carbide nanowire to the field of modified chlorinated polyethylene rubber to be used as a substitute, so that the problems of high cost of carbon black byproducts and serious pollution in the use process are overcome, and the method becomes an urgent task.
Disclosure of Invention
According to the interface modified chlorinated polyethylene rubber based on the novel reinforcing agent and the preparation method thereof, the boron carbide nanowires and the graphene are bonded together to obtain the graphene-coated boron carbide nanowires, so that the dispersibility of the nanowires in a matrix is enhanced, and the strength and the toughness of the rubber composite material are obviously improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
an interface modified chlorinated polyethylene rubber based on a novel reinforcing agent comprises the following raw materials in parts by weight: 80 parts of chlorinated polyethylene, 10 parts of reinforcing agent, 5 parts of coupling agent, 25 parts of flame retardant, 10 parts of stabilizer, 2 parts of auxiliary stabilizer, 1.5 parts of lubricant, 6 parts of halogen-free plasticizer, 3 parts of vulcanizing agent and 2 parts of vulcanizing assistant;
the reinforcing agent is a nano filler, the nano filler is a boron carbide nanowire, and the boron carbide nanowire is obtained by heating a mixture of a carbon nanotube and boron powder by using the carbon nanotube as a template;
the coupling agent is graphene, and the graphene is a high-quality graphene sheet and is directly made of graphite;
the stabilizer is the combination of magnesium oxide, zinc glycerolate and magnesium stearate.
Preferably, the flame retardant is a combination of a flame retardant of aluminum hydroxide and a flame retardant of antimony trioxide, wherein the flame retardant comprises 15 parts of aluminum hydroxide and 10 parts of antimony trioxide.
Preferably, the stabilizing agent comprises 6 parts of magnesium oxide, 2 parts of stabilizing agent zinc glycerolate and 2 parts of stabilizing agent magnesium stearate.
Preferably, the auxiliary stabilizer is a water-based epoxy resin.
Preferably, the lubricant is a microcrystalline wax.
Preferably, the halogen-free plasticizer is dioctyl phthalate serving as a plasticizer.
Preferably, the vulcanizing agent is dicumyl peroxide.
The invention also provides a preparation method of the interface modified chlorinated polyethylene rubber based on the novel reinforcing agent, which comprises the following steps:
(1) pretreating a reinforcing agent and a coupling agent: mixing and stirring the boron carbide nanowires and the graphene in an aqueous solution, enabling the boron carbide nanowires and the graphene to be bonded together by stirring, and freeze-drying to obtain graphene-coated boron carbide nanowires; the pre-coupling can firstly enhance the action of the reinforcing agent nanowire and the coupling agent, and is beneficial to the dispersibility of the nanowire in the rubber matrix;
(2) pouring powdery chlorinated polyethylene into a rubber mixing mill and mixing into sheets;
(3) adding a stabilizer and an auxiliary stabilizer, uniformly mixing, adding a flame retardant, a lubricant and a plasticizer, and uniformly mixing;
(4) then adding a mixture of a reinforcing agent and a coupling agent;
(5) and finally, opening the rubber mixing machine, adding a vulcanizing agent and a vulcanizing assistant when the temperature is lower than 90 ℃, and uniformly mixing to obtain a crude rubber finished product.
Compared with the prior art, the invention has the beneficial effects that:
(1) the nano filler is an ideal reinforcing material, can realize the combination of strength and toughness, and can obviously improve the strength, elastic modulus and fracture strain of the rubber material when added into the rubber material; the bending strength and the elastic modulus of the nano filler are increased along with the increase of the nano filler;
(2) the graphene can improve the interface problem between the filler and the matrix, improve the dispersion of the nano filler and the interface effect of the filler and the matrix, ensure that the dispersibility of the filler is more uniform, and improve the load transfer efficiency from the matrix to the reinforcing material, thereby improving the overall mechanical property of the rubber material;
(3) the base material, the coupling agent, the reinforcing agent and the stabilizing agent in the formula are safe and environment-friendly, do not contain substances which are harmful to the environment greatly, and follow the development trend of green chemistry.
Drawings
FIG. 1 is a diagram of nanowire encapsulation according to the present invention;
FIG. 2 is a graph of bending stress-strain curves for different amounts of coupling agent in accordance with the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In the description of the present invention, "a plurality" means two or more unless otherwise specified; the terms "upper", "lower", "left", "right", "inner", "outer", "front", "rear", "head", "tail", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, should not be construed as limiting the invention. Furthermore, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected" and "connected" are to be interpreted broadly, e.g., as being fixed or detachable or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1-2, an interface modified chlorinated polyethylene rubber based on a novel reinforcing agent comprises the following raw materials by weight: 80 parts of chlorinated polyethylene, 10 parts of reinforcing agent, 5 parts of coupling agent, 25 parts of flame retardant, 10 parts of stabilizer, 2 parts of auxiliary stabilizer, 1.5 parts of lubricant, 6 parts of halogen-free plasticizer, 3 parts of vulcanizing agent and 2 parts of vulcanizing assistant.
The rubber formula comprises the following specific raw materials in percentage by weight: 80 parts of chlorinated polyethylene, 10 parts of reinforcing agent boron carbide nanowire, 5 parts of coupling agent graphene, 15 parts of flame retardant aluminum hydroxide, 10 parts of flame retardant antimony trioxide, 6 parts of stabilizer magnesium oxide, 2 parts of stabilizer zinc glycerolate, 2 parts of stabilizer magnesium stearate, 2 parts of auxiliary stabilizer aqueous epoxy resin, 1.5 parts of lubricant microcrystalline wax, 6 parts of plasticizer dioctyl phthalate, 3 parts of vulcanizing agent dicumyl peroxide and 2 parts of vulcanizing agent triacrylate isocyanurate.
The boron carbide nanowire 2 as the reinforcing agent is obtained by heating a mixture of a carbon nanotube and boron powder by using the carbon nanotube as a template.
The graphene sheet 1 with high quality of the coupling agent is directly made of graphite.
The invention also provides a preparation method of the interface modified chlorinated polyethylene rubber based on the novel reinforcing agent, which comprises the following steps:
(1) pretreating a reinforcing agent and a coupling agent: mixing and stirring the boron carbide nanowire 2 and the graphene 1 in an aqueous solution, enabling the two to be bonded together by stirring, and freeze-drying to obtain a graphene-coated boron carbide nanowire 3; the pre-coupling can firstly enhance the action of the reinforcing agent nanowire and the coupling agent, and is beneficial to the dispersibility of the nanowire in the rubber matrix;
(2) pouring powdery chlorinated polyethylene into a rubber mixing mill and mixing into sheets;
(3) adding a stabilizer and an auxiliary stabilizer, uniformly mixing, adding a flame retardant, a lubricant and a plasticizer, and uniformly mixing;
(4) then adding a mixture of a reinforcing agent and a coupling agent;
(5) and finally, opening the rubber mixing machine, adding a vulcanizing agent and a vulcanizing assistant when the temperature is lower than 90 ℃, and uniformly mixing to obtain a crude rubber finished product.
The nanowire coating scheme of the present invention is shown in fig. 1.
The technical scheme adopts the combination of three stabilizers and one auxiliary stabilizer, namely the stabilizer magnesium oxide, the stabilizer zinc glycerolate, the stabilizer magnesium stearate and the auxiliary stabilizer epoxy resin, and the stabilizers and the auxiliary stabilizer are adopted because the stabilizers can play a stabilizing role in the whole rubber system, are green and nontoxic, can be used for applying the graphene-coated boron carbide nanowires to the field of modified chlorinated polyethylene rubber and serving as substitutes, and solves the problems of high cost and serious pollution in the production process of carbon black.
The specific reasons are as follows:
the effect of the stabilizer magnesium oxide in the modified chlorinated polyethylene rubber has three points:
firstly, magnesium oxide is added into a rubber product and can be used as an adsorbent to absorb free compounds generated by rubber vulcanization, so that the color of the product is more uniform and purer;
the addition of magnesium oxide can be used as an anti-reversion agent, so that the reversion tendency of the silk ribbon is flattened, and the crosslinking degree is improved;
thirdly, in the rubber type chlorinated polyethylene adhesive, the addition amount of magnesium oxide is larger, so that the magnesium oxide is used for absorbing hydrogen chloride gas generated in the processing and vulcanizing process and is a heat stabilizer with high quality and low price;
because the modified chlorinated polyethylene rubber has no double bond and no point of a cross-linking structure, the modified chlorinated polyethylene rubber is completely cross-linked by peroxide, and the high temperature during vulcanization promotes the peroxide to decompose to generate free radicals, so that the hydrogen on long-chain molecules of the modified chlorinated polyethylene rubber is captured, and the free radicals of the modified chlorinated polyethylene rubber are generated.
The stabilizer of zinc glycerolate has the following functions in the modified chlorinated polyethylene rubber: the thermal stability is improved.
The effect of the stabilizer magnesium stearate in the modified chlorinated polyethylene rubber is as follows: has good lubricating, anti-sticking, flow-aiding and dispersing functions. And the magnesium stearate and the zinc glycerolate have good synergistic effect, and when the compounding mass ratio of the magnesium stearate to the zinc glycerolate is 1:1, the thermal stability is fully exerted.
The epoxy resin is an important auxiliary heat stabilizer in production and processing, and is used for improving the heat resistance and the weather resistance of the stabilizer. They can absorb hydrogen chloride and replace unstable chlorine atoms in chlorinated polyethylene under the action of metal saponification so as to play the role of a stabilizer. The epoxy resin and the magnesium stearate have a synergistic effect, and the thermal stability of the chlorinated polyethylene can be improved.
According to the technical scheme, a stabilizer magnesium oxide, a stabilizer zinc glycerolate, a stabilizer magnesium stearate and an auxiliary stabilizer epoxy resin are combined together for the first time to serve as a composite stabilizer. The novel coupling agent and reinforcing agent mixture obtained by bonding the composite stabilizer, the boron carbide nanowires and the graphene together, namely the graphene-coated boron carbide nanowires, is applied to the field of modified chlorinated polyethylene rubber, and has an important effect. On one hand, under the action of the composite stabilizer, the anti-reversion agent, the adsorptivity, the thermal stability and the flow-aid lubrication dispersion function of the composite stabilizer are all improved, and the graphene-coated boron carbide nanowires are favorably used as novel reinforcing fillers to be applied to modified chlorinated polyethylene rubber (and the functions can be realized so as to realize the field application); on the other hand, the composite stabilizer is combined with the graphene-coated boron carbide nanowire to a certain degree, so that the interface problem is reduced. As shown in FIG. 2, the bending stress-strain curves of the product with different coupling agent dosages finally pass performance test detection, and the product is put into practical production application.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (9)
1. The interface modified chlorinated polyethylene rubber based on the novel reinforcing agent is characterized by comprising the following raw materials in parts by weight: 80 parts of chlorinated polyethylene, 10 parts of reinforcing agent, 5 parts of coupling agent, 25 parts of flame retardant, 10 parts of stabilizer, 2 parts of auxiliary stabilizer, 1.5 parts of lubricant, 6 parts of halogen-free plasticizer, 3 parts of vulcanizing agent and 2 parts of vulcanizing assistant;
the reinforcing agent is a nano filler, the nano filler is a boron carbide nanowire, and the boron carbide nanowire is obtained by heating a mixture of a carbon nanotube and boron powder by using the carbon nanotube as a template;
the coupling agent is graphene, and the graphene is a high-quality graphene sheet and is directly made of graphite;
the stabilizer is the combination of magnesium oxide, zinc glycerolate and magnesium stearate.
2. The novel reinforcing agent-based interface modified chlorinated polyethylene rubber as claimed in claim 1, wherein the flame retardant is a combination of flame retardant aluminum hydroxide and flame retardant antimony trioxide, wherein the flame retardant comprises 15 parts of flame retardant aluminum hydroxide and 10 parts of flame retardant antimony trioxide.
3. The novel reinforcing agent-based interface modified chlorinated polyethylene rubber as claimed in claim 1, wherein the stabilizer comprises 6 parts of magnesium oxide, 2 parts of zinc glycerolate and 2 parts of magnesium stearate.
4. The novel reinforcing agent-based interface-modified chlorinated polyethylene rubber as claimed in claim 1, wherein the auxiliary stabilizer is an aqueous epoxy resin.
5. The novel reinforcing agent-based interface-modified chlorinated polyethylene rubber as claimed in claim 1, wherein the lubricant is microcrystalline wax.
6. The novel reinforcing agent-based interface-modified chlorinated polyethylene rubber as claimed in claim 1, wherein the halogen-free plasticizer is dioctyl phthalate as a plasticizer.
7. The novel reinforcing agent-based interface modified chlorinated polyethylene rubber as claimed in claim 1, wherein the vulcanizing agent is dicumyl peroxide.
8. The novel reinforcing agent-based interface-modified chlorinated polyethylene rubber as claimed in claim 1, wherein the vulcanization aid is triacrylate isocyanurate.
9. A method for preparing an interface modified chlorinated polyethylene rubber based on a novel reinforcing agent according to any one of claims 1 to 8, comprising the following steps:
(1) firstly, pretreating a reinforcing agent and a coupling agent: mixing and stirring the boron carbide nanowires and the graphene in an aqueous solution, enabling the boron carbide nanowires and the graphene to be bonded together by stirring, and freeze-drying to obtain graphene-coated boron carbide nanowires; the pre-coupling can firstly enhance the action of the reinforcing agent nanowire and the coupling agent, and is beneficial to the dispersibility of the nanowire in the rubber matrix;
(2) pouring powdery chlorinated polyethylene into a rubber mixing mill and mixing into sheets;
(3) adding a stabilizer and an auxiliary stabilizer, uniformly mixing, adding a flame retardant, a lubricant and a plasticizer, and uniformly mixing;
(4) then adding a mixture of a reinforcing agent and a coupling agent;
(5) and finally, opening the rubber mixing machine, adding a vulcanizing agent and a vulcanizing assistant when the temperature is lower than 90 ℃, and uniformly mixing to obtain a crude rubber finished product.
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| CN202011271783.9A CN112358693A (en) | 2020-11-13 | 2020-11-13 | Interface modified chlorinated polyethylene rubber based on novel reinforcing agent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116554617A (en) * | 2023-06-12 | 2023-08-08 | 博硕科技(江西)有限公司 | Antimony-free flame-retardant polyvinyl chloride cable material, preparation method thereof and cable |
| US11970610B2 (en) | 2021-12-09 | 2024-04-30 | The Goodyear Tire & Rubber Company | Tire rubber composition using pyrazalone-based compound |
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| CN105038228A (en) * | 2015-08-03 | 2015-11-11 | 铜陵市胜达电子科技有限责任公司 | Polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for capacitor and preparation method thereof |
| CN111205529A (en) * | 2020-03-03 | 2020-05-29 | 山东菲纳科技发展有限公司 | Novel composite wear-resistant material for sucker rod elevator and preparation method thereof |
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2020
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Patent Citations (3)
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| JPS56131649A (en) * | 1980-03-21 | 1981-10-15 | Showa Denko Kk | Neutron shield |
| CN105038228A (en) * | 2015-08-03 | 2015-11-11 | 铜陵市胜达电子科技有限责任公司 | Polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for capacitor and preparation method thereof |
| CN111205529A (en) * | 2020-03-03 | 2020-05-29 | 山东菲纳科技发展有限公司 | Novel composite wear-resistant material for sucker rod elevator and preparation method thereof |
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| POLAT ET AL: "Microstructure and synergistic reinforcing activity of GNPs-B4C dual-micro and nano supplements in Al-Si matrix composites", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11970610B2 (en) | 2021-12-09 | 2024-04-30 | The Goodyear Tire & Rubber Company | Tire rubber composition using pyrazalone-based compound |
| CN116554617A (en) * | 2023-06-12 | 2023-08-08 | 博硕科技(江西)有限公司 | Antimony-free flame-retardant polyvinyl chloride cable material, preparation method thereof and cable |
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