CN113061294A - Preparation method and preparation device of graphene reinforced rubber - Google Patents
Preparation method and preparation device of graphene reinforced rubber Download PDFInfo
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- CN113061294A CN113061294A CN202110416543.1A CN202110416543A CN113061294A CN 113061294 A CN113061294 A CN 113061294A CN 202110416543 A CN202110416543 A CN 202110416543A CN 113061294 A CN113061294 A CN 113061294A
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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
- C08L7/00—Compositions of natural rubber
- C08L7/02—Latex
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B13/00—Conditioning or physical treatment of the material to be shaped
- B29B13/06—Conditioning or physical treatment of the material to be shaped by drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/002—Methods
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7476—Systems, i.e. flow charts or diagrams; Plants
- B29B7/748—Plants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7476—Systems, i.e. flow charts or diagrams; Plants
- B29B7/7495—Systems, i.e. flow charts or diagrams; Plants for mixing rubber
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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
- 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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses aThe preparation method of the graphene reinforced rubber comprises the following steps: preparing raw materials, preparing a mixed solution and preparing reinforced rubber; the thermal conductivity and mechanical strength of the prepared rubber are improved by adding the graphene, and a large amount of-NH is contained in the molecular chain of the dendritic polyamidoamine dendrimer2And the-CONH-polar group enables the rubber to have good water solubility, so that the mixing reaction speed is improved, the graphene is modified, so that the insulativity and the flame retardance of the rubber are improved, the synergistic effect of the graphene and other fillers is improved, the heat conductivity coefficient of the rubber is further improved, the aging of a polymer in the rubber is prevented and the service life of the rubber is prolonged by adding an antioxidant, the vulcanization promotion effect is exerted in the preparation process through zinc oxide, and the comprehensive performance of the rubber is improved.
Description
Technical Field
The invention relates to the technical field of rubber production and processing, in particular to a preparation method and a preparation device of graphene reinforced rubber.
Background
The rubber is a high-elasticity polymer material with reversible deformation, is widely applied to various aspects of industry or life, has elasticity at room temperature, can generate larger deformation under the action of small external force, and can recover the original shape after the external force is removed, the rubber belongs to a completely amorphous polymer, the glass transition temperature of the rubber is low, the molecular weight is often very large and is more than hundreds of thousands, the rubber is divided into two types, namely natural rubber and synthetic rubber, the natural rubber is prepared by extracting colloid from plants such as rubber trees, rubber grass and the like and then processing, the synthetic rubber is obtained by polymerizing various monomers, the reinforced rubber with higher comprehensive performance can be prepared by adding a reinforcing material in the preparation process of the rubber, and the reinforced rubber is widely applied to products such as automobile tires, hoses, conveyor belts and the like due to the excellent performance of the reinforced rubber;
the traditional reinforced rubber has single preparation raw materials, so that the prepared reinforced rubber can not meet the use requirements of the market gradually in comprehensive properties such as strength, toughness and the like, and the traditional reinforced rubber does not have good heat-conducting property and insulating property, so that the application of the reinforced rubber to electronic equipment is limited.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method and a preparation device of graphene reinforced rubber, the preparation method improves the thermal conductivity and mechanical strength of the prepared rubber by adding graphene powder in the preparation process, the graphene is modified by a surfactant and silicon dioxide, so that the insulativity and flame retardance of the reinforced rubber are improved, the synergistic effect of the graphene and other fillers in the preparation process of the rubber is improved, the heat conductivity coefficient of the rubber is further improved, the aging of polymers in the rubber is prevented and the service life of the rubber is prolonged by adding an antioxidant, the vulcanization promotion effect is exerted in the preparation process of the zinc oxide, the comprehensive performance of the rubber is improved, and the prepared graphene reinforced rubber can meet strict use requirements.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme: a preparation method of graphene reinforced rubber comprises the following steps:
the method comprises the following steps: raw material preparation
Weighing the following raw materials in parts by weight: 10-20 parts of graphene powder, 100-120 parts of deionized water, 8-12 parts of dendritic polyamidoamine, 5-10 parts of silicon dioxide, 5-10 parts of surfactant, 110-130 parts of natural rubber emulsion, 5-10 parts of zinc oxide and 4-8 parts of antioxidant;
step two: preparation of the Mixed solution
According to the first step, adding specified parts by weight of dendritic polyamidoamine, silicon dioxide, a surfactant, graphene powder and deionized water into a low-speed stirrer for mixing and stirring, reacting to obtain a modified graphene aqueous solution, directly polymerizing the modified graphene aqueous solution and a natural rubber emulsion, and mixing, stirring and uniformly dispersing a polymer by an ultrasonic dispersion machine to obtain a mixed solution;
step three: preparation of reinforced rubber
According to the second step, drying the mixed solution to obtain a mixed glue solution, adding the zinc oxide, the antioxidant and the mixed glue solution in the specified weight parts into a mixing device for mixing, and obtaining the graphene reinforced rubber after mixing.
The further improvement lies in that: in the first step, the raw materials are weighed according to the following parts by weight: 10 parts of graphene powder, 100 parts of deionized water, 8 parts of dendritic polyamidoamine, 5 parts of silicon dioxide, 5 parts of surfactant, 110 parts of natural rubber emulsion, 5 parts of zinc oxide and 4 parts of antioxidant.
The further improvement lies in that: in the first step, the raw materials are weighed according to the following parts by weight: 20 parts of graphene powder, 120 parts of deionized water, 12 parts of dendritic polyamidoamine, 10 parts of silicon dioxide, 10 parts of surfactant, 130 parts of natural rubber emulsion, 10 parts of zinc oxide and 8 parts of antioxidant.
The further improvement lies in that: in the first step, the graphene powder is prepared by a mechanical stripping method, and the surfactant is an anionic surfactant.
The further improvement lies in that: in the first step, the main component of the natural rubber emulsion is cis-1, 4-polyisoprene, and the antioxidant is peroxide decomposition type antioxidant.
The further improvement lies in that: and in the fourth step, the mixed solution is dried by a drying box, the heating temperature of the mixed solution in the drying box is set to be 100 ℃, and the drying time is 30 minutes.
The utility model provides a preparation facilities of graphite alkene reinforcing rubber, includes mixed solution preparation facilities and rubber preparation facilities, mixed solution preparation facilities includes low-speed mixer and ultrasonic dispersion machine, rubber preparation facilities includes stoving case and mixing equipment.
The invention has the beneficial effects that: according to the invention, the graphene is added in the preparation process, so that the thermal conductivity and the mechanical strength of the prepared rubber are improved, and a large amount of-NH is contained in the molecular chain of the dendritic polyamidoamine dendrimer2And the-CONH-polar group enables the graphene to have good water solubility, so that the mixing reaction speed is improved, the graphene is subjected to modification treatment through the surfactant and the silicon dioxide, so that the insulativity and the flame retardance of the reinforced rubber are improved, and the performance of the graphene and other fillers in the rubber preparation process is improvedThe heat conductivity coefficient of the rubber is further improved through the synergistic effect, the aging of polymers in the rubber is prevented and the service life of the rubber is prolonged through the addition of the antioxidant, the prepared graphene reinforced rubber can meet strict use requirements through the vulcanization promotion effect of zinc oxide in the preparation process and the comprehensive performance of the rubber is improved, and the graphene reinforced rubber can be widely applied to electronic equipment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of a preparation method of the present invention;
FIG. 2 is a schematic view of the structure of a manufacturing apparatus of 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. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," "fourth," 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 should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example one
Referring to fig. 1, the present embodiment provides a preparation method of graphene reinforced rubber, including the following steps:
the method comprises the following steps: raw material preparation
Weighing the following raw materials in parts by weight: the graphene-based composite material comprises, by weight, 10 parts of graphene powder, 100 parts of deionized water, 8 parts of dendritic polyamidoamine, 5 parts of silicon dioxide, 5 parts of a surfactant, 110 parts of a natural rubber emulsion, 5 parts of zinc oxide and 4 parts of an antioxidant, wherein the graphene powder is prepared by a mechanical stripping method, the surfactant is an anionic surfactant, the main component of the natural rubber emulsion is cis-1, 4-polyisoprene, and the antioxidant is a peroxide decomposition type antioxidant;
step two: preparation of the Mixed solution
According to the first step, adding specified parts by weight of dendritic polyamidoamine, silicon dioxide, a surfactant, graphene powder and deionized water into a low-speed stirrer for mixing and stirring, reacting to obtain a modified graphene aqueous solution, directly polymerizing the modified graphene aqueous solution and a natural rubber emulsion, and mixing, stirring and uniformly dispersing a polymer by an ultrasonic dispersion machine to obtain a mixed solution;
step three: preparation of reinforced rubber
According to the second step, firstly drying the mixed solution to obtain a mixed glue solution, then adding the zinc oxide, the antioxidant and the mixed glue solution in the specified weight parts into a mixing device for mixing, obtaining the graphene reinforced rubber after mixing, drying the mixed solution through a drying box, setting the heating temperature of the mixed solution in the drying box to be 100 ℃, and setting the drying time to be 30 minutes.
Referring to fig. 2, the embodiment provides a preparation apparatus for graphene reinforced rubber, which includes a mixed solution preparation apparatus and a rubber preparation apparatus, wherein the mixed solution preparation apparatus includes a low-speed stirrer and an ultrasonic disperser, and the rubber preparation apparatus includes a drying box and a mixing device.
Example two
Referring to fig. 1, the present embodiment provides a preparation method of graphene reinforced rubber, including the following steps:
the method comprises the following steps: raw material preparation
Weighing the following raw materials in parts by weight: the graphene-based composite material comprises, by weight, 20 parts of graphene powder, 120 parts of deionized water, 12 parts of dendritic polyamidoamine, 10 parts of silicon dioxide, 10 parts of a surfactant, 130 parts of a natural rubber emulsion, 10 parts of zinc oxide and 8 parts of an antioxidant, wherein the graphene powder is prepared by a mechanical stripping method, the surfactant is an anionic surfactant, the main component of the natural rubber emulsion is cis-1, 4-polyisoprene, and the antioxidant is a peroxide decomposition type antioxidant;
step two: preparation of the Mixed solution
According to the first step, adding specified parts by weight of dendritic polyamidoamine, silicon dioxide, a surfactant, graphene powder and deionized water into a low-speed stirrer for mixing and stirring, reacting to obtain a modified graphene aqueous solution, directly polymerizing the modified graphene aqueous solution and a natural rubber emulsion, and mixing, stirring and uniformly dispersing a polymer by an ultrasonic dispersion machine to obtain a mixed solution;
step three: preparation of reinforced rubber
According to the second step, firstly drying the mixed solution to obtain a mixed glue solution, then adding the zinc oxide, the antioxidant and the mixed glue solution in the specified weight parts into a mixing device for mixing, obtaining the graphene reinforced rubber after mixing, drying the mixed solution through a drying box, setting the heating temperature of the mixed solution in the drying box to be 100 ℃, and setting the drying time to be 30 minutes.
Referring to fig. 2, the embodiment provides a preparation apparatus for graphene reinforced rubber, which includes a mixed solution preparation apparatus and a rubber preparation apparatus, wherein the mixed solution preparation apparatus includes a low-speed stirrer and an ultrasonic disperser, and the rubber preparation apparatus includes a drying box and a mixing device.
The dendritic polyamidoamine in the graphene reinforced rubber has the effects of increasing dispersibility, increasing solubility, improving the dissolution amount of effective components, reducing mixing requirements by reducing viscosity, improving fluidity and wettability, and increasing interaction with the surfaces of various materials because reaction groups on the outer layer of dendritic molecules can provide polyions;
the dendritic polyamidoamine has a large number of end groups, can be subjected to different functional modification, can be well used as a carrier of graphene, can be used as a high-degree dispersing agent and a stabilizing agent, and is used for synthesizing nanoparticles;
in addition, the molecular chain of the dendritic polyamidoamine dendrimer contains a large amount of-NH 2 and-CONH-polar groups, so that the dendrimer has good water solubility, and a large amount of terminal groups of the dendrimer are easy to perform functional modification, such as low viscosity, high double-bond functionality and high reaction speed of a hyperbranched polymer of which the terminal group contains a double-bond group;
cavities and a large number of surface functional groups exist in a highly branched molecular structure in the dendritic polyamidoamine, so that the dendritic polyamidoamine is not easy to crystallize and easy to form a film, has low melt viscosity and solution viscosity and incomparable nanometer characteristics, and also has excellent dissolving and dispersing properties;
the dendritic polymer added in the preparation process has the structural characteristics and excellent characteristics that the center has a core, the interior has a cavity, a large number of branching units are arranged, modifiable functional groups are uniformly distributed on the surface, the volume, the shape, the functional groups and the molecular weight can be accurately controlled at the molecular level, the dendritic polymer is highly branched, has a regular and delicate perfect structure, is spherical at a high generation number, and has a nano-scale size as a raw material, good solubility and low viscosity.
The graphene reinforced rubber obtained in each example was subjected to a correlation performance test, and the test results are shown in table 1.
Table 1 results of performance testing
According to the preparation method of the graphene reinforced rubber, the graphene is added in the preparation process, so that the thermal conductivity and the mechanical strength of the prepared rubber are improved, and a molecular chain of a dendritic polyamidoamine dendrimer contains a large amount of-NH2And the-CONH-polar group enables the graphene reinforced rubber to have good water solubility, so that the mixing reaction speed is improved, the graphene is modified by the surfactant and the silicon dioxide, so that the insulativity and the flame retardance of the reinforced rubber are improved, the synergistic effect of the graphene and other fillers in the rubber preparation process is improved, the heat conductivity coefficient of the rubber is further improved, the aging of polymers in the rubber is prevented and the service life of the rubber is prolonged by adding the antioxidant, the vulcanization promotion effect is exerted in the preparation process of the zinc oxide, the comprehensive performance of the rubber is improved, so that the prepared graphene reinforced rubber can meet strict use requirements, and can be widely applied to electronic equipment.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of graphene reinforced rubber is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: raw material preparation
Weighing the following raw materials in parts by weight: 10-20 parts of graphene powder, 100-120 parts of deionized water, 8-12 parts of dendritic polyamidoamine, 5-10 parts of silicon dioxide, 5-10 parts of surfactant, 110-130 parts of natural rubber emulsion, 5-10 parts of zinc oxide and 4-8 parts of antioxidant;
step two: preparation of the Mixed solution
According to the first step, adding specified parts by weight of dendritic polyamidoamine, silicon dioxide, a surfactant, graphene powder and deionized water into a low-speed stirrer for mixing and stirring, reacting to obtain a modified graphene aqueous solution, directly polymerizing the modified graphene aqueous solution and a natural rubber emulsion, and mixing, stirring and uniformly dispersing a polymer by an ultrasonic dispersion machine to obtain a mixed solution;
step three: preparation of reinforced rubber
According to the second step, drying the mixed solution to obtain a mixed glue solution, adding the zinc oxide, the antioxidant and the mixed glue solution in the specified weight parts into a mixing device for mixing, and obtaining the graphene reinforced rubber after mixing.
2. The method for preparing graphene reinforced rubber according to claim 1, wherein the method comprises the following steps: in the first step, the raw materials are weighed according to the following parts by weight: 10 parts of graphene powder, 100 parts of deionized water, 8 parts of dendritic polyamidoamine, 5 parts of silicon dioxide, 5 parts of surfactant, 110 parts of natural rubber emulsion, 5 parts of zinc oxide and 4 parts of antioxidant.
3. The method for preparing graphene reinforced rubber according to claim 1, wherein the method comprises the following steps: in the first step, the raw materials are weighed according to the following parts by weight: 20 parts of graphene powder, 120 parts of deionized water, 12 parts of dendritic polyamidoamine, 10 parts of silicon dioxide, 10 parts of surfactant, 130 parts of natural rubber emulsion, 10 parts of zinc oxide and 8 parts of antioxidant.
4. The method for preparing graphene reinforced rubber according to claim 1, wherein the method comprises the following steps: in the first step, the graphene powder is prepared by a mechanical stripping method, and the surfactant is an anionic surfactant.
5. The method for preparing graphene reinforced rubber according to claim 1, wherein the method comprises the following steps: in the first step, the main component of the natural rubber emulsion is cis-1, 4-polyisoprene, and the antioxidant is peroxide decomposition type antioxidant.
6. The method for preparing graphene reinforced rubber according to claim 1, wherein the method comprises the following steps: and in the fourth step, the mixed solution is dried by a drying box, the heating temperature of the mixed solution in the drying box is set to be 100 ℃, and the drying time is 30 minutes.
7. The utility model provides a preparation facilities of graphite alkene reinforcing rubber, includes mixed solution preparation facilities and rubber preparation facilities, its characterized in that: the mixed solution preparation device comprises a low-speed stirrer and an ultrasonic dispersion machine, and the rubber preparation device comprises a drying box and mixing equipment.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102390830A (en) * | 2011-08-23 | 2012-03-28 | 华南理工大学 | Method for preparing polyamide-amine in-situ intercalation graphene composite material |
| US20140323610A1 (en) * | 2012-02-23 | 2014-10-30 | Beijing University Of Chemical Technology | Method for preparing graphene oxide/white carbon black/rubber nanocomposite material |
| CN110577675A (en) * | 2018-06-07 | 2019-12-17 | 山东欧铂新材料有限公司 | Graphene/silicon dioxide/natural rubber composite material and preparation method and application thereof |
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- 2021-04-19 CN CN202110416543.1A patent/CN113061294A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102390830A (en) * | 2011-08-23 | 2012-03-28 | 华南理工大学 | Method for preparing polyamide-amine in-situ intercalation graphene composite material |
| US20140323610A1 (en) * | 2012-02-23 | 2014-10-30 | Beijing University Of Chemical Technology | Method for preparing graphene oxide/white carbon black/rubber nanocomposite material |
| CN110577675A (en) * | 2018-06-07 | 2019-12-17 | 山东欧铂新材料有限公司 | Graphene/silicon dioxide/natural rubber composite material and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
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| 李勇，等: "《废旧高分子材料循环利用》", 31 July 2019, 冶金工业出版社 * |
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