CN108164663A - A kind of graphene enhancing ethylene propylene diene rubber and preparation method thereof - Google Patents
A kind of graphene enhancing ethylene propylene diene rubber and preparation method thereof Download PDFInfo
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- CN108164663A CN108164663A CN201711445404.1A CN201711445404A CN108164663A CN 108164663 A CN108164663 A CN 108164663A CN 201711445404 A CN201711445404 A CN 201711445404A CN 108164663 A CN108164663 A CN 108164663A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/14—Organic medium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/68—Vanadium, niobium, tantalum or compounds thereof
Abstract
The invention discloses a kind of graphenes to enhance ethylene propylene diene rubber, is formed including following parts by weight：
Description
Technical field
The present invention relates to chemical technology field, more specifically, it relates to a kind of graphene enhancing ethylene propylene diene rubber and
Preparation method.
Background technology
Ethylene propylene diene rubber (EPDM) is the rubber formed by ethylene, propylene through solution copolymerization, is re-introduced into Third monomer.
Ethylene propylene diene rubber is substantially a kind of high polymer of saturation, is the synthetic rubber of high comprehensive performance, is had fabulous electrical
Can, ageing properties.But due to being free of crystalline solid, so intensity is very low, the scope of application is very restricted.
In order to improve the intensity of EPDM materials, fiber is commonly used to enhance EPDM.Most studied in recent years is to use nylon
(PA) its tearing strength and tensile strength are improved to EPDM enhancings, the research to the formula and vulcanization process of EPDM-PA systems
It is 52 to show EPDM and PA proportionings:When 35, EPDM materials reach better mechanical property.In addition, recently studies have found that with three
The fibre-reinforced EPDM materials of poly cyanamid have good tensile strength, but also show the processing characteristics of plastics.But these
Enhancements are all to carry out strength improving again on the basis of synthetic EPDM, not to it from the preparation process of EPDM
It is improved.
Graphene is the two dimension crystalline substance of only one layer atomic thickness for being stripped out from graphite material, being made of carbon atom
Body is had excellent mechanical property and is widely used in the humidification of all kinds of organic and inorganic materials, increased using graphene
Strong EPDM also has relevant report, but be to add graphene again on synthetic EPDM to be modified, and graphene is straight
It scoops out and is had not been reported in the synthesis of EPDM.
Invention content
Increase graphene from synthesis the object of the present invention is to provide one kind and improve ethylene propylene diene rubber intensity, so as to obtain
Ethylene propylene diene rubber of high intensity and preparation method thereof.
The first object of the present invention is to provide a kind of graphene enhancing ethylene propylene diene rubber.
To achieve the above object, it is realized by following technological means：
A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
Advanced optimize for：A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
Advanced optimize for：A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
Advanced optimize for：The Third monomer is polybutadiene rubber of the 1,2- polybutadiene contents more than 9%
Or the polyisoprene rubber of 3,4- polyisoprene more than 9% or both combination.
Advanced optimize for：The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, described
Vanadium series catalyst be VOCl3、VO(P204)2、V(acac)3、VOCl3·nMOH、VO2Cl (trioctylamine), VO2Cl33 (phosphorus
Sour tributyl), VO (OH) (8-hydroxy-quinoline)2Or VO (OH) (ɑ-cupron)2One or more of combination, wherein M
For the alkyl of C5~C8,2.5≤n≤3.5；The alkyl aluminum compound is trimethyl aluminium, triethyl aluminum, ethylaluminum two
The combination of one or more of aluminium, ethyl aluminum dichloride, aluminium diethyl monochloride or dichloro aluminium isobutyl；The activation accelerating agent is
Ethyl trichloroacetate, CH3Cl、CH2Cl2Or CHCl3One or more of combination.
Advanced optimize for：The organic solvent is the saturated alkane of C5~C10.
Advanced optimize for：The terminator is sodium dimethyl dithiocarbamate, in sodium polysulfide, sodium nitrite
One or more combination.
Advanced optimize for：The stabilizer is lead sulfate tribasic, dibasic lead phosphite, dibasic lead stearate
One or more of combination.
Advanced optimize for：The reducing agent is sodium borohydride or potassium borohydride or both combination.
The second object of the present invention is to provide a kind of preparation method of graphene enhancing ethylene propylene diene rubber.
To achieve the above object, it is realized by following technological means：A kind of preparation of graphene enhancing ethylene propylene diene rubber
Method includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, graphene oxide, catalysis
Agent, organic solvent are added in reaction kettle, are passed through ethylene and propylene mixed gas into reaction kettle, and setting pressure 0.5~
1.8MPa, 40~60 DEG C of temperature react 40~50min under the atmosphere of logical hydrogen stream, obtain the first colloidal solution.
(3) ash disposal：Stabilizer is added in the first colloidal solution of gained into (2), normal temperature and pressure reacts 50~60min,
Up to the second colloidal solution；
(4) it restores：Add in reducing agent into (3) in second colloidal solution of gained, 40~80 DEG C are reacted 4~6 hours, i.e.,
Obtain third colloidal solution；
(5) precipitation：The third colloidal solution of gained in (4) is transferred in flocculate tank, control pressure 0.35~
0.45MPa, 80~95 DEG C of temperature remove solvent after flocculation, obtain colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
The advantages of the present invention over the prior art are that：The active oxygen atom group of surface of graphene oxide, such as hydroxyl
(- OH), carboxyl (- COOH), carbonyl (- C=OH) etc., and the rough surface of graphene oxide.Graphene oxide is added into
Into environment existing for ethylene, propylene and Third monomer, graphene oxide can pass through the active group and Third monomer on surface
Grafting effect occurs, and Third monomer on the other hand can be with ethylene, propylene polymerization, so graphene oxide is grafted on third list
On the polymer formed after body and ethylene, propylene polymerization, formed by the polymer architecture of graphene oxide weave in, then
In subsequent reduction process, graphene oxide is reduced into graphene, is formed by the polymer architecture of graphene weave in,
Graphene oxide is lamellar structure, and after being grafted with Third monomer, Third monomer combination ethylene, propylene can be grafted on graphene oxide
Upper and lower surface, after graphene oxide is reduced into graphene, Third monomer combination ethylene, propylene be still in graphene up and down
Surface forms the composite construction that lamellar graphite alkene is mixed between polymer, poly- in addition to tearing when external force is wanted to tear rubber
Beyond the region of objective existence is closed, the graphene of stratiform is also torn, along with the very high substance of inherently a kind of intensity of graphene so that composite junction
The tensile strength and fracture strength of structure are all very high, can promote the integral strength of polymer, finally obtain the EPDM of high intensity
Rubber.
Specific embodiment
Invention is described in further detail below by specific embodiment, following embodiment is descriptive, is not to limit
Protection scope of the present invention of property.
Embodiment 1
A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
The Third monomer is polybutadiene rubber of the 1,2- polybutadiene contents 9%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VOCl3, the alkyl aluminum compound is trimethyl aluminium, and the activation accelerating agent is ethyl trichloroacetate.
The organic solvent is hexane.
The terminator is sodium dimethyl dithiocarbamate.
The stabilizer is lead sulfate tribasic.
The reducing agent is sodium borohydride.
A kind of preparation method of graphene enhancing ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, graphene oxide, catalysis
Agent, organic solvent are added in reaction kettle, and ethylene and propylene mixed gas are passed through into reaction kettle, set pressure 0.5MPa, temperature
40 DEG C of degree reacts 40min under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 50min to get
Second colloidal solution；
(4) it restores：Reducing agent is added in the second colloidal solution of gained into (3), 40 DEG C are reacted 4 hours to get third
Colloidal solution；
(5) precipitation：The third colloidal solution of gained in (4) is transferred in flocculate tank, control pressure 0.35MPa, temperature
80 DEG C, solvent is removed after flocculation, obtains colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 2
A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
The Third monomer is polyisoprene rubber of the 3,4- polyisoprene 9%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VO (P204)2, the alkyl aluminum compound is triethyl aluminum, and the activation accelerating agent is CH3Cl。
The organic solvent is octane.
The terminator is sodium polysulfide.
The stabilizer is dibasic lead phosphite.
The reducing agent is potassium borohydride.
A kind of preparation method of graphene enhancing ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, graphene oxide, catalysis
Agent, organic solvent are added in reaction kettle, and ethylene and propylene mixed gas are passed through into reaction kettle, set pressure 1.8MPa, temperature
60 DEG C of degree reacts 50min under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 60min to get
Second colloidal solution；
(4) it restores：Reducing agent is added in the second colloidal solution of gained into (3), 80 DEG C are reacted 6 hours to get third
Colloidal solution；
(5) precipitation：The third colloidal solution of gained in (4) is transferred in flocculate tank, control pressure 0.45MPa, temperature
95 DEG C, solvent is removed after flocculation, obtains colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 3
A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
The Third monomer is polybutadiene rubber of the 1,2- polybutadiene contents more than 16%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For V (acac)3, the alkyl aluminum compound is two aluminium of ethylaluminum, and the activation accelerating agent is CH2Cl2。
The organic solvent is pentane.
The terminator is sodium nitrite.
The stabilizer is dibasic lead stearate.
Combination of the reducing agent for sodium borohydride and potassium borohydride.
A kind of preparation method of graphene enhancing ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, graphene oxide, catalysis
Agent, organic solvent are added in reaction kettle, and ethylene and propylene mixed gas are passed through into reaction kettle, set pressure 0.8MPa, temperature
42 DEG C of degree reacts 42min under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 55min to get
Second colloidal solution；
(4) it restores：Reducing agent is added in the second colloidal solution of gained into (3), 50 DEG C are reacted 5 hours to get third
Colloidal solution；
(5) precipitation：The third colloidal solution of gained in (4) is transferred in flocculate tank, control pressure 0.37MPa, temperature
82 DEG C, solvent is removed after flocculation, obtains colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 4
A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
The Third monomer is polyisoprene rubber of the 3,4- polyisoprene 15%.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VOCl3·3C5H12OH, the alkyl aluminum compound are ethyl aluminum dichloride, and the activation accelerating agent is trichloroacetic acid second
Ester and CH3The combination of Cl.
The organic solvent is heptane.
The terminator is sodium polysulfide.
The stabilizer is dibasic lead phosphite.
The reducing agent is potassium borohydride.
A kind of preparation method of graphene enhancing ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, graphene oxide, catalysis
Agent, organic solvent are added in reaction kettle, and ethylene and propylene mixed gas are passed through into reaction kettle, set pressure 1.2MPa, temperature
46 DEG C of degree reacts 46min under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 58min to get
Second colloidal solution；
(4) it restores：Add in reducing agent into (3) in second colloidal solution of gained, 70 DEG C of reactions 5.4 hours are to get the
Three colloidal solutions；
(5) precipitation：The third colloidal solution of gained in (4) is transferred in flocculate tank, control pressure 0.39MPa, temperature
90 DEG C, solvent is removed after flocculation, obtains colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Embodiment 5
A kind of graphene enhances ethylene propylene diene rubber, is formed including following parts by weight：
The Third monomer is polybutadiene rubber and 3,4- poly- isoamyl of the 1,2- polybutadiene contents more than 12%
Diene 13% polyisoprene rubber combination.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VO2Cl33 (tributyl phosphates), the alkyl aluminum compound are aluminium diethyl monochloride, and the activation accelerating agent is
CH2Cl2With CH3The combination of Cl.
The organic solvent is octane.
Combination of the terminator for sodium dimethyl dithiocarbamate and sodium polysulfide.
Combination of the stabilizer for lead sulfate tribasic and dibasic lead phosphite.
The reducing agent is sodium borohydride.
A kind of preparation method of graphene enhancing ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, graphene oxide, catalysis
Agent, organic solvent are added in reaction kettle, and ethylene and propylene mixed gas are passed through into reaction kettle, set pressure 1.8MPa, temperature
48 DEG C of degree reacts 48min under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 55min to get
Second colloidal solution；
(4) it restores：Reducing agent is added in the second colloidal solution of gained into (3), 48 DEG C are reacted 5 hours to get third
Colloidal solution；
(5) precipitation：The third colloidal solution of gained in (4) is transferred in flocculate tank, control pressure 0.42MPa, temperature
85 DEG C, solvent is removed after flocculation, obtains colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Comparative example 1
A kind of ethylene propylene diene rubber is formed including following parts by weight：
The Third monomer is polybutadiene rubber and 3,4- poly- isoamyl of the 1,2- polybutadiene contents more than 16%
Diene 15% polyisoprene rubber combination.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VO (OH) (8-hydroxy-quinoline)2, the alkyl aluminum compound is dichloro aluminium isobutyl, and the activation accelerating agent is three
Ethyl chloroacetate and CHCl3Combination.
The organic solvent is nonane.
Combination of the terminator for sodium dimethyl dithiocarbamate and sodium nitrite.
Combination of the stabilizer for lead sulfate tribasic and dibasic lead stearate.
A kind of preparation method of ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, catalyst, organic solvent
It is added in reaction kettle, ethylene and propylene mixed gas is passed through into reaction kettle, pressure 0.58MPa, temperature 50 C, logical are set
50min is reacted under the atmosphere of hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 53min to get
Second colloidal solution；
(4) precipitation：Second colloidal solution of gained in (3) is transferred in flocculate tank, control pressure 0.45MPa, temperature
90 DEG C, solvent is removed after flocculation, obtains colloid；
(5) it is dry：The colloid of gained in (4) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Comparative example 2
A kind of ethylene propylene diene rubber is formed including following parts by weight：
The Third monomer is polybutadiene rubber and 3,4- poly- isoamyl of the 1,2- polybutadiene contents more than 14%
Diene 17% polyisoprene rubber combination.
The catalyst includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, the vanadium series catalyst
For VO (OH) (ɑ-cupron)2, the alkyl aluminum compound is the combination of trimethyl aluminium and dichloro aluminium isobutyl, described
Activation accelerating agent be CH2Cl2With CH3The combination of Cl.
The organic solvent is decane.
Combination of the terminator for sodium polysulfide and sodium nitrite.
Combination of the stabilizer for dibasic lead phosphite and dibasic lead stearate.
A kind of preparation method of ethylene propylene diene rubber, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, catalyst, organic solvent
It is added in reaction kettle, ethylene and propylene mixed gas is passed through into reaction kettle, pressure 0.5MPa, 40 DEG C of temperature, logical are set
40min is reacted under the atmosphere of hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 57min to get
Second colloidal solution；
(4) precipitation：Second colloidal solution of gained in (3) is transferred in flocculate tank, control pressure 0.35MPa, temperature
80 DEG C, solvent is removed after flocculation, obtains colloid；
(5) it is dry：The colloid of gained in (4) is dehydrated through dewaterer, drying machine drying is to get final EPDM
Rubber.
Ethylene propylene diene rubber obtained by above-described embodiment and comparative example is tested into its draftability according to GB/T528-1998
Can, test result is as shown in table 1.
By data in table it is found that being added to graphene after, the tensile strength of ethylene propylene diene rubber is greatly improved,
The intensity enhancing of i.e. entire ethylene propylene diene rubber.
The tensile property of ethylene propylene diene rubber obtained by 1 embodiment and comparative example of table
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of graphene enhances ethylene propylene diene rubber, which is characterized in that is formed including following parts by weight：
2. a kind of graphene enhances ethylene propylene diene rubber, which is characterized in that is formed including following parts by weight：
3. a kind of graphene enhances ethylene propylene diene rubber, which is characterized in that is formed including following parts by weight：
A kind of 4. graphene enhancing ethylene propylene diene rubber according to any one of claim 1 to 3, which is characterized in that institute
The Third monomer stated for polybutadiene rubber of the 1,2- polybutadiene contents more than 9% or 3,4- polyisoprene 9% with
On polyisoprene rubber or both combination.
A kind of 5. graphene enhancing ethylene propylene diene rubber according to any one of claim 1 to 3, which is characterized in that institute
The catalyst stated includes vanadium series catalyst, alkyl aluminum compound and activation accelerating agent, and the vanadium series catalyst is VOCl3、VO
(P204)2、V(acac)3、VOCl3·nMOH、VO2Cl (trioctylamine), VO2Cl33 (tributyl phosphates), VO (OH) (eight hydroxyls
Base quinoline)2Or VO (OH) (ɑ-cupron)2One or more of combination, wherein M be C5~C8 alkyl, 2.5≤n≤
3.5；The alkyl aluminum compound is trimethyl aluminium, triethyl aluminum, two aluminium of ethylaluminum, ethyl aluminum dichloride, a chlorine diethyl
The combination of one or more of base aluminium or dichloro aluminium isobutyl；The activation accelerating agent is ethyl trichloroacetate, CH3Cl、
CH2Cl2Or CHCl3One or more of combination.
A kind of 6. graphene enhancing ethylene propylene diene rubber according to any one of claim 1 to 3, which is characterized in that institute
The organic solvent stated is the saturated alkane of C5~C10.
A kind of 7. graphene enhancing ethylene propylene diene rubber according to any one of claim 1 to 3, which is characterized in that institute
The terminator stated is the combination of one or more of sodium dimethyl dithiocarbamate, sodium polysulfide, sodium nitrite.
A kind of 8. graphene enhancing ethylene propylene diene rubber according to any one of claim 1 to 3, which is characterized in that institute
The stabilizer stated is the combination of one or more of lead sulfate tribasic, dibasic lead phosphite, dibasic lead stearate.
A kind of 9. graphene enhancing ethylene propylene diene rubber according to any one of claim 1 to 3, which is characterized in that institute
The reducing agent stated is sodium borohydride or potassium borohydride or both combination.
10. a kind of preparation method of graphene enhancing ethylene propylene diene rubber according to any one of claim 1 to 3,
It is characterized in that, includes the following steps：
(1) each raw material is weighed according to components by weight percent；
(2) it polymerize：Reaction kettle is sufficiently displaced from inert gas, by the Third monomer weighed, graphene oxide, catalyst,
Organic solvent is added in reaction kettle, and ethylene and propylene mixed gas are passed through into reaction kettle, sets 0.5~1.8MPa of pressure,
40~60 DEG C of temperature reacts 40~50min under the atmosphere of logical hydrogen stream, obtains the first colloidal solution.
(3) ash disposal：Add in stabilizer into (2) in first colloidal solution of gained, normal temperature and pressure react 50~60min to get
Second colloidal solution；
(4) it restores：Add in reducing agent into (3) in second colloidal solution of gained, 40~80 DEG C of reactions 4~6 hours are to get the
Three colloidal solutions；
(5) precipitation：The third colloidal solution of gained in (4) is transferred in flocculate tank, 0.35~0.45MPa of control pressure, temperature
80~95 DEG C of degree removes solvent after flocculation, obtains colloid；
(6) it is dry：The colloid of gained in (5) is dehydrated through dewaterer, drying machine drying is to get final ethylene-propylene-diene monomer
Glue.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109206820A (en) * | 2018-08-13 | 2019-01-15 | 中铁二院工程集团有限责任公司 | A kind of ageing-resistant EPT rubber packing material and preparation method thereof |
| CN109713173A (en) * | 2018-12-06 | 2019-05-03 | 深圳市量能科技有限公司 | A kind of anode nut cap, preparation method and battery |
| CN114874394A (en) * | 2021-02-05 | 2022-08-09 | 中国石油化工股份有限公司 | Ethylene propylene diene monomer and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109206820A (en) * | 2018-08-13 | 2019-01-15 | 中铁二院工程集团有限责任公司 | A kind of ageing-resistant EPT rubber packing material and preparation method thereof |
| CN109206820B (en) * | 2018-08-13 | 2020-08-04 | 中铁二院工程集团有限责任公司 | Aging-resistant ethylene propylene diene monomer sealing material and preparation method thereof |
| CN109713173A (en) * | 2018-12-06 | 2019-05-03 | 深圳市量能科技有限公司 | A kind of anode nut cap, preparation method and battery |
| CN114874394A (en) * | 2021-02-05 | 2022-08-09 | 中国石油化工股份有限公司 | Ethylene propylene diene monomer and preparation method and application thereof |
| CN114874394B (en) * | 2021-02-05 | 2023-11-14 | 中国石油化工股份有限公司 | Ethylene propylene diene monomer rubber and preparation method and application thereof |
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