CN112300330A - Preparation method of ethylene propylene diene monomer rubber plate - Google Patents
Preparation method of ethylene propylene diene monomer rubber plate Download PDFInfo
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- CN112300330A CN112300330A CN202011147144.1A CN202011147144A CN112300330A CN 112300330 A CN112300330 A CN 112300330A CN 202011147144 A CN202011147144 A CN 202011147144A CN 112300330 A CN112300330 A CN 112300330A
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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
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
- C08F255/06—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms on to ethene-propene-diene terpolymers
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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
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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
- C08F253/00—Macromolecular compounds obtained by polymerising monomers on to natural rubbers or derivatives thereof
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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
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention belongs to the field of rubber, and particularly relates to a preparation method of ethylene propylene diene monomer, which comprises the following steps of: 30-60 parts of ethylene propylene diene monomer, 40-80 parts of natural rubber, 10-20 parts of maleic anhydride, 2-6 parts of initiator, 4-8 parts of vulcanizing agent, 1-3 parts of antioxidant and 14-20 parts of filler, and provides a specific preparation method. The invention solves the problem of high mixing difficulty of the ethylene propylene diene monomer, opens the side double bonds from the molecular level, and cooperates with the covalent bonds to form a network structure through chemical crosslinking, thereby improving the strength and toughness of the ethylene propylene diene monomer.
Description
Technical Field
The invention belongs to the field of rubber, and particularly relates to a preparation method of ethylene propylene diene monomer.
Background
The ethylene propylene diene monomer is saturated nonpolar rubber, has excellent chemical medium resistance, thermal oxidation aging resistance, heat and humidity cold resistance and electrical insulation, can be used for a long time at the temperature of-60-135 ℃, and has the advantages of minimum density, large filling property, low ablation rate, large specific heat and good comprehensive performance compared with other general rubbers. Therefore, the composite material is widely applied to the fields of aerospace, rail transit, automobiles, buildings, buffering packaging materials and the like, and the production and consumption are rapidly improved in recent years. However, ethylene propylene diene monomer is saturated rubber, the processing difficulty is high during mixing, a general sulfur vulcanization system is not suitable, the vulcanization time is long, and meanwhile, the compatibility of ethylene propylene diene monomer and other unsaturated rubber is poor, so that product delamination is easy to occur.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of an ethylene propylene diene monomer rubber plate, which solves the problem of high mixing difficulty of ethylene propylene diene monomer rubber, opens a side double bond from a molecular layer, and cooperates with a covalent bond to form a network structure through chemical crosslinking, thereby improving the strength and toughness of the ethylene propylene diene monomer rubber.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of an ethylene propylene diene monomer rubber plate comprises the following steps:
30-60 parts of ethylene propylene diene monomer, 40-80 parts of natural rubber, 10-20 parts of maleic anhydride, 2-6 parts of initiator, 4-8 parts of vulcanizing agent, 1-3 parts of antioxidant and 14-20 parts of filler.
The initiator comprises a main initiator dicumyl peroxide.
Further, the initiator also comprises an auxiliary initiator, wherein the auxiliary initiator adopts styrene, and the using amount of the auxiliary initiator is 2-5% of the mass of the main initiator.
The vulcanizing agent adopts benzoyl peroxide or 2, 4-dichlorobenzoyl peroxide.
The antioxidant adopts antioxidant 1010.
The filler adopts nano titanium dioxide or nano silicon dioxide.
Furthermore, the nano titanium dioxide adopts anatase titanium dioxide with the particle size of 10-40 nm.
The preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder to be ground, and uniformly stirring to form a mixture, wherein the grinding pressure is 2-5MPa, and the temperature is 20-40 ℃;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin, wherein the mixing temperature is 170 ℃, the mixing stirring speed is 1000-1500r/min, and the mixing time is 10-30 min;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer; wherein the mixing temperature is 160 ℃, the mixing stirring speed is 500-;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding and molding to prepare the ethylene propylene diene monomer rubber plate, wherein the vulcanizing temperature is 160 ℃, the pressure is 10MPa, and the time is 60-90 min.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the problem of high mixing difficulty of the ethylene propylene diene monomer, opens the side double bonds from the molecular level, and cooperates with the covalent bonds to form a network structure through chemical crosslinking, thereby improving the strength and toughness of the ethylene propylene diene monomer.
2. The invention utilizes the mixing of the initiator, the ethylene propylene diene monomer, the natural rubber and the maleic anhydride and the characteristic of easy grafting of the maleic anhydride to graft the initiator on double bonds of the ethylene propylene diene monomer and the natural rubber, thereby improving the problem of poor compatibility.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
Example 1
The preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder to be ground, and uniformly stirring to form a mixture, wherein the grinding pressure is 2MPa, and the temperature is 20 ℃;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin, wherein the mixing temperature is 170 ℃, the mixing stirring speed is 1000r/min, and the mixing time is 10 min;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer; wherein the mixing temperature is 160 ℃, the mixing stirring speed is 500r/min, and the mixing time is 10 min;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding to form the ethylene propylene diene monomer rubber plate, wherein the vulcanizing temperature is 160 ℃, the pressure is 10MPa, and the time is 60 min.
Wherein the mass ratio is as follows:
30g of ethylene propylene diene monomer, 40g of natural rubber, 10g of maleic anhydride, 2g of initiator, 4g of vulcanizing agent, 1g of antioxidant and 14g of filler;
the initiator comprises a main initiator dicumyl peroxide.
The vulcanizing agent adopts benzoyl peroxide.
The antioxidant adopts antioxidant 1010.
The filler is nano titanium dioxide.
Example 2
The preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder to be ground, and uniformly stirring to form a mixture, wherein the grinding pressure is 5MPa, and the temperature is 40 ℃;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin, wherein the mixing temperature is 170 ℃, the mixing stirring speed is 1500r/min, and the mixing time is 30 min;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer; wherein the mixing temperature is 160 ℃, the mixing stirring speed is 1000r/min, and the mixing time is 30 min;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding and molding to prepare the ethylene propylene diene monomer rubber plate, wherein the vulcanizing temperature is 160 ℃, the pressure is 10MPa, and the time is 90 min.
Wherein the mass ratio is as follows:
60g of ethylene propylene diene monomer, 80g of natural rubber, 20g of maleic anhydride, 6g of initiator, 8g of vulcanizing agent, 3g of antioxidant and 20g of filler;
the initiator comprises a main initiator dicumyl peroxide.
The vulcanizing agent adopts 2, 4-dichlorobenzoyl peroxide.
The antioxidant adopts antioxidant 1010.
The filler adopts nano silicon dioxide.
Example 3
The preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder to be ground, and uniformly stirring to form a mixture, wherein the grinding pressure is 4MPa, and the temperature is 30 ℃;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin, wherein the mixing temperature is 170 ℃, the mixing stirring speed is 1400r/min, and the mixing time is 15 min;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer; wherein the mixing temperature is 160 ℃, the mixing stirring speed is 800r/min, and the mixing time is 20 min;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding and molding to prepare the ethylene propylene diene monomer rubber plate, wherein the vulcanizing temperature is 160 ℃, the pressure is 10MPa, and the time is 70 min.
Wherein the mass ratio is as follows:
50g of ethylene propylene diene monomer, 60g of natural rubber, 15g of maleic anhydride, 4g of initiator, 6g of vulcanizing agent, 2g of antioxidant and 17g of filler;
the initiator comprises a main initiator dicumyl peroxide.
The vulcanizing agent adopts benzoyl peroxide.
The antioxidant adopts antioxidant 1010.
The filler is nano titanium dioxide.
Example 4
The preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder to be ground, and uniformly stirring to form a mixture, wherein the grinding pressure is 3MPa, and the temperature is 25 ℃;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin, wherein the mixing temperature is 170 ℃, the mixing stirring speed is 1300r/min, and the mixing time is 20 min;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer; wherein the mixing temperature is 160 ℃, the mixing stirring speed is 800r/min, and the mixing time is 20 min;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding to form the ethylene propylene diene monomer rubber plate, wherein the vulcanizing temperature is 160 ℃, the pressure is 10MPa, and the time is 80 min.
Wherein the mass ratio is as follows:
50g of ethylene propylene diene monomer, 60g of natural rubber, 15g of maleic anhydride, 4g of initiator, 6g of vulcanizing agent, 2g of antioxidant and 18g of filler;
the initiator comprises a main initiator dicumyl peroxide and an auxiliary initiator which adopts styrene, and the usage amount of the auxiliary initiator is 2 percent of the mass of the main initiator.
The vulcanizing agent adopts benzoyl peroxide.
The antioxidant adopts antioxidant 1010.
The filler is nano titanium dioxide, and the nano titanium dioxide is anatase titanium dioxide with the particle size of 10 nm.
Example 5
The preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder to be ground, and uniformly stirring to form a mixture, wherein the grinding pressure is 5MPa, and the temperature is 40 ℃;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin, wherein the mixing temperature is 170 ℃, the mixing stirring speed is 1500r/min, and the mixing time is 30 min;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer; wherein the mixing temperature is 160 ℃, the mixing stirring speed is 1000r/min, and the mixing time is 30 min;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding and molding to prepare the ethylene propylene diene monomer rubber plate, wherein the vulcanizing temperature is 160 ℃, the pressure is 10MPa, and the time is 90 min.
Wherein the mass ratio is as follows:
30g of ethylene propylene diene monomer, 40g of natural rubber, 10g of maleic anhydride, 2g of initiator, 4g of vulcanizing agent, 1g of antioxidant and 14g of filler;
the initiator comprises a main initiator dicumyl peroxide and an auxiliary initiator which adopts styrene, and the usage amount of the auxiliary initiator is 5 percent of the mass of the main initiator.
The vulcanizing agent adopts benzoyl peroxide.
The antioxidant adopts antioxidant 1010.
The filler is nano titanium dioxide, and the nano titanium dioxide is anatase titanium dioxide with the particle size of 40 nm.
Example 6
The preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder to be ground, and uniformly stirring to form a mixture, wherein the grinding pressure is 2MPa, and the temperature is 20 ℃;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin, wherein the mixing temperature is 170 ℃, the mixing stirring speed is 1000r/min, and the mixing time is 10 min;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer; wherein the mixing temperature is 160 ℃, the mixing stirring speed is 500r/min, and the mixing time is 10 min;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding to form the ethylene propylene diene monomer rubber plate, wherein the vulcanizing temperature is 160 ℃, the pressure is 10MPa, and the time is 60 min.
Wherein the mass ratio is as follows:
30g of ethylene propylene diene monomer, 40g of natural rubber, 10g of maleic anhydride, 2g of initiator, 4g of vulcanizing agent, 1g of antioxidant and 14g of filler;
the initiator comprises a main initiator dicumyl peroxide and an auxiliary initiator which adopts styrene, and the usage amount of the auxiliary initiator is 4% of the mass of the main initiator.
The vulcanizing agent adopts 2, 4-dichlorobenzoyl peroxide.
The antioxidant adopts antioxidant 1010.
The filler is nano titanium dioxide, and the nano titanium dioxide is anatase titanium dioxide with the particle size of 30 nm.
Performance detection
The tensile strength and elongation at break of samples 1-6 and the comparative samples obtained in the above examples are shown in the following table:
wherein, the comparative example is a commercial ethylene propylene diene monomer rubber plate
In summary, the invention has the following advantages:
1. the invention solves the problem of high mixing difficulty of the ethylene propylene diene monomer, opens the side double bonds from the molecular level, and cooperates with the covalent bonds to form a network structure through chemical crosslinking, thereby improving the strength and toughness of the ethylene propylene diene monomer.
2. The invention utilizes the mixing of the initiator, the ethylene propylene diene monomer, the natural rubber and the maleic anhydride and the characteristic of easy grafting of the maleic anhydride to graft the initiator on double bonds of the ethylene propylene diene monomer and the natural rubber, thereby improving the problem of poor compatibility.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (10)
1. A preparation method of an ethylene propylene diene monomer rubber plate is characterized by comprising the following steps: the mass ratio is as follows:
30-60 parts of ethylene propylene diene monomer, 40-80 parts of natural rubber, 10-20 parts of maleic anhydride, 2-6 parts of initiator, 4-8 parts of vulcanizing agent, 1-3 parts of antioxidant and 14-20 parts of filler.
2. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 1, wherein the method comprises the following steps: the initiator comprises a main initiator dicumyl peroxide.
3. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 1, wherein the method comprises the following steps: the vulcanizing agent adopts benzoyl peroxide or 2, 4-dichlorobenzoyl peroxide.
4. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 1, wherein the method comprises the following steps: the antioxidant adopts antioxidant 1010.
5. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 1, wherein the method comprises the following steps: the filler adopts nano titanium dioxide or nano silicon dioxide.
6. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 1, wherein the method comprises the following steps: the preparation method of the ethylene propylene diene monomer rubber plate comprises the following steps:
step 1, adding ethylene propylene diene monomer, natural rubber and maleic anhydride into a grinder for grinding, and uniformly stirring to form a mixture;
step 2, adding the mixture and an initiator into mixing equipment for mixing to obtain mixed crosslinked resin;
step 3, adding the mixed crosslinked resin and an antioxidant into a reaction kettle for mixing to obtain modified ethylene propylene diene monomer;
and 4, adding a vulcanizing agent and a filler into the reaction kettle, uniformly stirring, vulcanizing, and extruding and molding to obtain the ethylene propylene diene monomer rubber plate.
7. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 6, wherein the method comprises the following steps: the crushing pressure in the step 1 is 2-5MPa, and the temperature is 20-40 ℃.
8. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 6, wherein the method comprises the following steps: the mixing temperature in the step 2 is 170 ℃, the mixing stirring speed is 1500r/min and the mixing time is 10-30 min.
9. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 6, wherein the method comprises the following steps: the mixing temperature in the step 3 is 160 ℃, the mixing stirring speed is 500-1000r/min, and the mixing time is 10-30 min.
10. The method for preparing the ethylene propylene diene monomer rubber sheet according to claim 6, wherein the method comprises the following steps: the temperature of the vulcanization treatment in the step 4 is 160 ℃, the pressure is 10MPa, and the time is 60-90 min.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB883524A (en) * | 1957-06-18 | 1961-11-29 | Montedison Spa | Improved elastomers and their preparation |
| US3884882A (en) * | 1973-01-10 | 1975-05-20 | Du Pont | Certain EPDM copolymer/maleic anhydride adducts and thermoplastic elastomers therefrom |
| US4687810A (en) * | 1986-01-02 | 1987-08-18 | Monsanto Company | Making rubber blends of diene rubber & EPR or EPDM |
| CN107022148A (en) * | 2017-06-06 | 2017-08-08 | 镇江瑞科化工有限公司 | A kind of resistant to elevated temperatures rubber composition |
-
2020
- 2020-10-23 CN CN202011147144.1A patent/CN112300330A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB883524A (en) * | 1957-06-18 | 1961-11-29 | Montedison Spa | Improved elastomers and their preparation |
| US3884882A (en) * | 1973-01-10 | 1975-05-20 | Du Pont | Certain EPDM copolymer/maleic anhydride adducts and thermoplastic elastomers therefrom |
| US4687810A (en) * | 1986-01-02 | 1987-08-18 | Monsanto Company | Making rubber blends of diene rubber & EPR or EPDM |
| CN107022148A (en) * | 2017-06-06 | 2017-08-08 | 镇江瑞科化工有限公司 | A kind of resistant to elevated temperatures rubber composition |
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