CN107641176B - Rubber composition and preparation method of rubber material - Google Patents
Rubber composition and preparation method of rubber material Download PDFInfo
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Abstract
The invention discloses a rubber composition and a preparation method of a rubber material, and belongs to the field of rubber. The rubber composition comprises rubber, methacrylic acid, montmorillonite modified by a cationic surfactant, a vulcanizing agent and an anti-aging agent. The rubber composition improves the internal stress transfer capacity of rubber through the interaction of an electrostatic interface, double bond combination or physical winding and the like, achieves the aim of further improving the rubber performance by using a small amount of nano filler, and avoids the problems that the rubber performance cannot meet the use requirement by using a small amount of nano filler, and the nano filler is more in material, so that the nano filler is easy to agglomerate, thereby causing the reduction of the reinforcing force.
Description
Technical Field
The invention relates to the field of rubber, in particular to a rubber composition and a preparation method of a rubber material.
Background
In order to improve the performance of rubber, it is generally necessary to knead and vulcanize rubber with additives such as vulcanizing agents and fillers.
Currently, commonly used rubber fillers include carbon black, calcium carbonate, mica, china clay, montmorillonite, carbon nanotubes, graphene, and the like. The nano-fillers such as montmorillonite, carbon nano-tube and graphene can play an obvious role in reinforcing rubber under the condition of small volume filling amount.
However, when the rubber performance needs to be further improved, due to the high specific surface area of the nano-filler, after a certain amount of the nano-filler is filled in the rubber, the nano-filler is converged and integrated into a large nano-aggregate or aggregated into a larger micron-sized form, so that the stress transfer capability of the nano-filler is seriously reduced, the reinforcing capability is reduced, and the rubber performance cannot be better improved even if the amount of the filler is increased.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a rubber composition and a preparation method of a rubber material, wherein the rubber composition enables an electrostatic interface, double bond combination or physical winding and other interactions to exist between montmorillonite/rubber, the internal stress transfer capability between the rubber and the montmorillonite is greatly improved, the purpose of further improving the rubber performance by using a small amount of nano-filler is realized, and the problems that the rubber performance cannot meet the use requirement due to the small amount of the nano-filler and the reinforcing force is reduced due to the agglomeration easily caused by the large amount of the nano-filler are solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a rubber composition comprises rubber, methacrylic acid, montmorillonite modified by cationic surfactant, vulcanizing agent and anti-aging agent.
In an optional embodiment, the rubber composition comprises the following components in parts by mass:
100 parts of rubber, 10-30 parts of methacrylic acid, 5-15 parts of montmorillonite modified by a cationic surfactant, 1-6 parts of a vulcanizing agent and 1-3 parts of an anti-aging agent.
In an optional embodiment, the rubber is one or more of acrylonitrile butadiene rubber or hydrogenated acrylonitrile butadiene rubber with the mass content of acrylonitrile being 18-45%.
In an alternative embodiment, the surface modifier used in the cationic surfactant modified montmorillonite is CH3(CH2)17NH2、CH3(CH2)17NHCOCH(CH3)＝CHCH＝CH(CH3)COOMn+Wherein M is one or more of the combinationsn+Is Na+、Mg2+、Zn2+、Ca2+Or Al3+。
In an alternative embodiment, the vulcanizing agent is one or a combination of two of dicumyl peroxide and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane.
In an optional embodiment, the anti-aging agent is one or more of amine and phenol anti-aging agents.
A preparation method of a rubber material comprises the following steps:
step 1, mixing methacrylic acid and montmorillonite modified by a cationic surfactant to prepare slurry;
obtaining mixed rubber;
and 3, vulcanizing the rubber compound to obtain the rubber material.
In an optional embodiment, the components in the steps 1 and 2 are mixed according to the following mass parts:
100 parts of rubber, 10-30 parts of methacrylic acid, 5-15 parts of montmorillonite modified by a cationic surfactant, 1-6 parts of a vulcanizing agent and 1-3 parts of an anti-aging agent.
In an optional embodiment, the rubber in the step 2 is one or more of acrylonitrile butadiene rubber or hydrogenated acrylonitrile butadiene rubber with the acrylonitrile mass content of 18-45%;
the surface modifier used by the montmorillonite modified by the cationic surfactant in the step 1 is CH3(CH2)17NH2Or CH3(CH2)17NHCOCH(CH3)＝CHCH＝CH(CH3)COOMn+Wherein M is one or more of the combinationsn+Is Na+、Mg2+、Zn2+、Ca2+Or Al3+；
The vulcanizing agent in the step 2 is one or two combinations of dicumyl peroxide and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane;
the anti-aging agent in the step 2 is one or a combination of more than one of amine and phenol anti-aging agents.
In an alternative embodiment, the mixing the masticated rubber and the slurry in step 2 comprises:
and mixing the plasticated rubber with the slurry at 90-110 ℃ for not less than 5 min.
In an alternative embodiment, before adding the vulcanizing agent and the anti-aging agent and mixing in step 2, the method further comprises:
and cooling the mixed nitrile rubber and the slurry to below 40 ℃.
In an alternative embodiment, the vulcanization in step 3 is carried out at a temperature of 140 to 170 ℃ and a pressure of 5 to 15 MPa.
The invention has the following advantages:
in the rubber composition provided by the embodiment of the invention, methacrylic acid forms polymethacrylic acid after being initiated by a vulcanizing agent, and in the initiating process, the methacrylic acid can react with double bonds in a rubber main molecular chain on one hand and graft the polymethacrylic acid on the rubber molecular chain on the other hand, the methacrylic acid which is graft polymerized on the rubber molecular chain can also provide carboxyl to form ion pairs with a cationic surfactant on the surface of montmorillonite, so that the binding force between montmorillonite filler and the polymethacrylic acid is enhanced; because the grafted polymethacrylic acid is combined with a rubber molecular chain through a chemical bond or physically intertwined together, an electrostatic interface, double bond combination or physical intertwining and other interactions exist between the montmorillonite and the rubber, the internal stress transfer capability between the rubber and the montmorillonite is greatly improved, the purpose that the rubber performance can be further improved by using a small amount of nano-filler is realized, and the problems that the rubber performance cannot meet the use requirement due to the small amount of the nano-filler, and the nano-filler is easy to agglomerate due to the large amount of the nano-filler, so that the reinforcing force is reduced are solved;
the rubber composition provided by the embodiment of the invention is mainly prepared from common chemical substances, is nontoxic and harmless, has low cost and is beneficial to popularization and application;
the preparation method of the rubber composition provided by the invention has the advantages of conventional equipment, simple process and strong operability.
Drawings
FIG. 1 is an SEM image of a rubber material provided in example 1 of the present invention;
FIG. 2 is a tensile hysteresis curve at 200% elongation of the rubber materials provided in example 1 of the present invention and comparative example 1.
Detailed Description
The invention is further illustrated by the following specific examples:
the embodiment of the invention provides a rubber composition which comprises rubber, methacrylic acid (2-methacrylic acid), montmorillonite modified by a cationic surfactant, a vulcanizing agent and an anti-aging agent.
In the rubber composition provided by the embodiment of the invention, methacrylic acid forms polymethacrylic acid after being initiated by a vulcanizing agent, and in the initiating process, the methacrylic acid can react with double bonds in a rubber main molecular chain on one hand and graft the polymethacrylic acid on the rubber molecular chain on the other hand, the methacrylic acid which is graft polymerized on the rubber molecular chain can also provide carboxyl to form ion pairs with a cationic surfactant on the surface of montmorillonite, so that the binding force between montmorillonite filler and the polymethacrylic acid is enhanced; because the grafted polymethacrylic acid and a rubber molecular chain are combined together through a chemical bond or physically intertwined, an electrostatic interface, double bond combination or physical intertwining and other interactions exist between the montmorillonite and the rubber, the internal stress transfer capability between the rubber and the montmorillonite is greatly improved, the purpose that the rubber performance can be further improved by using a small amount of nano-filler is realized, and the problems that the rubber performance cannot meet the use requirement due to the small amount of the nano-filler, and the nano-filler is more in material consumption and is easy to agglomerate, so that the reinforcing force is reduced are solved.
In an alternative embodiment, the rubber composition comprises the following components in parts by mass: 100 parts of rubber, 10-30 parts of methacrylic acid, 5-15 parts of montmorillonite modified by a cationic surfactant, 1-6 parts of a vulcanizing agent and 1-3 parts of an anti-aging agent.
The rubber can be nitrile rubber, hydrogenated nitrile butadiene, ethylene propylene rubber, natural rubber and butadiene rubber, preferably nitrile rubber, more preferably one or more of nitrile rubber with the mass content of acrylonitrile being 18-45% or hydrogenated nitrile rubber; the surface modifier used for the montmorillonite modified by the cationic surfactant is preferably octadecylamine (CH)3(CH2)17NH2) Or octadecylamine and suberic acidAmong them, preferred is (CH)3(CH2)17NHCOCH(CH3)＝CHCH＝CH(CH3)COOMn+Wherein M is one or more of the combinationsn+Is Na+、Mg2+、Zn2+、Ca2+Or Al3+(ii) a The vulcanizing agent is preferably one or two combinations of dicumyl peroxide and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane; the anti-aging agent is preferably one or more of amine and phenol anti-aging agents.
Further, the rubber composition provided by the embodiment of the present invention may further include a rubber compounding agent such as a vulcanization aid, and the vulcanization aid is preferably one or a combination of more than one of triallyl cyanurate, triallyl isocyanurate, divinylbenzene, diallyl phthalate, trimethylolpropane trimethacrylate, and ethylene glycol dimethacrylate.
The embodiment of the invention also provides a preparation method of the rubber composition, which comprises the following steps:
step 1, mixing methacrylic acid and montmorillonite modified by a cationic surfactant to prepare slurry;
specifically, in the embodiment of the invention, methacrylic acid and montmorillonite modified by cationic surfactant are fully mixed in a kneader or a stirrer at normal temperature to prepare slurry;
specifically, in the embodiment of the invention, when the rubber is raw rubber, the rubber is plasticated to improve the rubber performance; after plastication, heating and mixing rubber and the slurry on an open mill for a certain time, then cooling to room temperature, and adding compounding agents such as an anti-aging agent, a vulcanizing agent and the like for mixing; after mixing, triangular bags are packed, and after the mixture is thinly passed for several times, the mixture is taken out to obtain mixed rubber;
and 3, vulcanizing the rubber compound to obtain the rubber material.
Specifically, in the embodiment of the present invention, the vulcanization can be performed by a conventional vulcanization process, and the vulcanization time can be determined according to the positive vulcanization time measured by a vulcanizer.
In the rubber material prepared by the preparation method of the rubber composition provided by the embodiment of the invention, methacrylic acid is initiated by a vulcanizing agent to form polymethacrylic acid, so that in the initiation process, the methacrylic acid can react with double bonds in a rubber main molecular chain to graft the polymethacrylic acid on the rubber molecular chain, and on the other hand, the methacrylic acid which is graft polymerized on the rubber molecular chain can also provide carboxyl to form ion pairs with a cationic surfactant on the surface of montmorillonite, so that the binding force between montmorillonite filler and the polymethacrylic acid is enhanced; because the grafted polymethacrylic acid and a rubber molecular chain are combined together through a chemical bond or physically intertwined, an electrostatic interface, double bond combination or physical intertwining and other interactions exist between the montmorillonite and the rubber, the internal stress transfer capability between the rubber and the montmorillonite is greatly improved, the purpose that the rubber performance can be further improved by using a small amount of nano-filler is realized, and the problems that the rubber performance cannot meet the use requirement due to the small amount of the nano-filler, and the nano-filler is more in material consumption and is easy to agglomerate, so that the reinforcing force is reduced are solved. Specifically, the components in the steps 1 and 2 are preferably mixed according to the following mass parts:
100 parts of rubber, 10-30 parts of methacrylic acid, 5-15 parts of montmorillonite modified by a cationic surfactant, 1-6 parts of a vulcanizing agent and 1-3 parts of an anti-aging agent.
The rubber can be nitrile rubber, ethylene propylene rubber, natural rubber and butadiene rubber, preferably nitrile rubber, more preferably one or more of nitrile rubber with the mass content of acrylonitrile being 18-45% or hydrogenated nitrile rubber; the surface modifier used for the montmorillonite modified by the cationic surfactant is preferably octadecylamine (CH)3(CH2)17NH2) Or condensation derivatives of octadecylamine and suberic acid, of which (CH) is preferred3(CH2)17NHCOCH(CH3)＝CHCH＝CH(CH3)COOMn+Wherein M is one or more of the combinationsn+Is Na+、Mg2+、Zn2+、Ca2+Or Al3+(ii) a The vulcanizing agent is preferably one or two combinations of dicumyl peroxide and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane; the antioxidant is preferably at least one of amine antioxidant and phenol antioxidant, such as antioxidant MB, antioxidant RD, antioxidant D, etc.
Further, the rubber composition provided by the embodiment of the present invention may further include a rubber compounding agent such as a vulcanization aid, and the vulcanization aid is preferably one or a combination of more than one of triallyl cyanurate, triallyl isocyanurate, divinylbenzene, diallyl phthalate, trimethylolpropane trimethacrylate, and ethylene glycol dimethacrylate.
Specifically, the mixing of the masticated rubber and the slurry in the step 2 includes:
and mixing the plasticated rubber with the slurry at 90-110 ℃ for not less than 5 min.
After high-temperature mixing, the viscosity of the rubber is reduced, so that the rubber can better perform intercalation or stripping on montmorillonite and the like, and a good nano dispersion effect is formed.
Further, before adding the vulcanizing agent and the anti-aging agent and mixing in the step 2, the method further comprises the following steps:
and cooling the mixed nitrile rubber and the slurry to below 40 ℃.
Avoiding scorching of the rubber material after the vulcanizing agent is added at a higher temperature.
Specifically, the vulcanization in the step 3 is carried out at the temperature of 140-170 ℃ and the pressure of 5-15 MPa for mold pressing, and the vulcanization time can be determined according to the positive vulcanization time tested by a vulcanization instrument.
The following are several specific embodiments of the invention:
in the following examples, the surface-modified montmorillonite used in example 1 was I.31ps from commercial Nanocro; example 2 is Nanocro I.31ps and HOOCCH (CH)3)＝CHCH＝CH(CH3) COOH (mass ratio 1: 1) dehydrating and condensing at 120 ℃, and adjusting the pH to 8-9 by using sodium hydroxide; example 3 Nanocro I.31ps and HOOCCH (CH)3)＝CHCH＝CH(CH3) COOH (mass ratio 1: 1) dehydrating and condensing at 120 ℃, and adjusting the pH to 8-9 by using magnesium hydroxide; example 4 is I.31ps from Nanocro.
Example 1:
step (1), weighing 100g of nitrile rubber (the content of acrylonitrile is 18 percent), 15g of 2-methacrylic acid and CH3(CH2)17NH25g of surface modified montmorillonite, 3g of dicumyl peroxide, 1g of anti-aging agent MB and 2g of anti-aging agent RD.
Step (2), weighing methacrylic acid and CH at normal temperature3(CH2)17NH2The surface modified montmorillonite is evenly mixed in a kneading machine to prepare slurry.
Plasticating the weighed nitrile rubber, and thermally mixing the sizing material and the slurry prepared in the step (2) for 8min on a 90 ℃ open mill after plastication; cooling the mixed rubber material to room temperature, sequentially adding the antioxidant MB, the antioxidant RD and dicumyl peroxide weighed in the step (1), and mixing on an open mill; and (5) making a triangular bag, thinly passing for several times, and then discharging the slices.
And (4) cutting the rubber material after sheet discharge into a certain shape, putting the rubber material into a mold, and vulcanizing the rubber material for 30min at 160 ℃ and 15MPa to obtain the rubber material.
FIG. 1 shows the dispersion of montmorillonite in the rubber material prepared in example 1, and FIG. 1 shows the dispersion of montmorillonite as C and the dispersion of polymethacrylic acid as D, and it can be seen from FIG. 1 that montmorillonite forms a good stripping/intercalation state in the rubber material, and polymethacrylic acid can be well connected to montmorillonite to form a strong interface, which is beneficial to rubber reinforcement.
Comparative example 1:
step (1), weighing 100g of nitrile butadiene rubber (acrylonitrile content is 18 percent), CH3(CH2)17NH25g of surface modified montmorillonite, 3g of dicumyl peroxide, 1g of anti-aging agent MB and 2g of anti-aging agent RD.
And (2) plasticating the weighed nitrile rubber, cooling to room temperature after plasticating, then sequentially adding the montmorillonite, the anti-aging agent and the vulcanizing agent weighed in the step (1) into the plasticated rubber, mixing on an open mill, packaging in a triangular bag, thinly passing for several times, and then discharging the sheet.
And (3) cutting the rubber material after sheet discharge into a certain shape, putting the rubber material into a mold, and vulcanizing the rubber material for 30min at 160 ℃ and 15MPa to obtain the rubber material.
Comparative example 2:
step (1), weighing 100g of nitrile rubber (the acrylonitrile content is 18%), 15g of 2-methacrylic acid, 3g of dicumyl peroxide, 1g of antioxidant MB and 2g of antioxidant RD.
And (2) plasticating the weighed nitrile rubber, cooling to room temperature after plasticating, then sequentially adding the 2-methacrylic acid anti-aging agent and the vulcanizing agent weighed in the step (1) into the plasticated rubber, mixing on an open mill, packaging in a triangular bag, thinly passing for several times, and then discharging the sheet.
And (3) cutting the rubber material after sheet discharge into a certain shape, putting the rubber material into a mold, and vulcanizing the rubber material for 30min at 160 ℃ and 15MPa to obtain the rubber material.
Example 2
Step (1), weighing 100g of hydrogenated nitrile-butadiene rubber (the content of acrylonitrile is 18 percent), 20g of 2-methacrylic acid and CH3(CH2)17NHCOCH(CH3)＝CHCH＝CH(CH3)COO-Na+5g of surface modified montmorillonite, 3g of dicumyl peroxide, 1g of anti-aging agent MB and 2g of anti-aging agent RD.
And (2) fully mixing the weighed methacrylic acid and the surface modified montmorillonite in a kneader at normal temperature to prepare slurry.
Plasticating the weighed nitrile rubber, and thermally mixing the sizing material and the slurry prepared in the step (2) for 7min on an open mill at 100 ℃ after plastication; and (3) cooling the mixed rubber material to room temperature, sequentially adding the anti-aging agent and the vulcanizing agent weighed in the step (1), mixing on an open mill, performing triangular packaging, performing thin passing for several times, and then discharging the sheet.
(4) Cutting the rubber material after sheet discharge into a certain shape, putting the rubber material into a mold, and vulcanizing the rubber material for 40min at the temperature of 150 ℃ and the pressure of 10MPa to obtain the rubber material.
Example 3
Step (1), weighing 100g of hydrogenated nitrile rubber (the content of acrylonitrile is 34 percent), 30g of 2-methacrylic acid, (CH)3(CH2)17NHCOCH(CH3)＝CHCH＝CH(CH3)COO-)2Mg2+10g of surface modified montmorillonite, 6g of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, 1g of anti-aging agent MB and 1.5g of triallyl isocyanurate.
And (2) fully mixing the methacrylic acid weighed in the step (1) and the surface modified montmorillonite in a kneader at normal temperature to prepare slurry.
Plasticating the hydrogenated nitrile-butadiene rubber weighed in the step (1), and thermally mixing the rubber material and the slurry prepared in the step (2) for 6min on an open mill at the temperature of 110 ℃ after plastication; and (3) cooling the mixed rubber material to room temperature, sequentially adding the anti-aging agent, the vulcanizing agent and the vulcanizing aid weighed in the step (1), mixing on an open mill, performing triangular packaging, performing thin passing for several times, and then discharging the sheet.
(4) Cutting the rubber material after sheet discharge into a certain shape, putting the rubber material into a mold, and vulcanizing for 10min at 170 ℃ and 10MPa to obtain the rubber material.
Example 4
Step (1), weighing 100g of nitrile rubber (the acrylonitrile content is 36-40%), 25g of 2-methacrylic acid and CH3(CH2)17NH215g of surface modified montmorillonite, 3g of dicumyl peroxide and 3g of anti-aging agent D.
And (2) fully mixing the methacrylic acid weighed in the step (1) and the surface modified montmorillonite in a kneader at normal temperature to prepare slurry.
Plasticating the weighed nitrile rubber, and thermally mixing the sizing material and the slurry prepared in the step (2) for 7min on an open mill at 100 ℃ after plastication; and (3) cooling the mixed rubber material to room temperature, sequentially adding the anti-aging agent and the vulcanizing agent weighed in the step (1), mixing on an open mill, performing triangular packaging, performing thin passing for several times, and then discharging the sheet.
And (4) cutting the rubber material after sheet discharge into a certain shape, putting the rubber material into a mold, and vulcanizing the rubber material for 40min at 140 ℃ and 5MPa to obtain the rubber material.
The rubber materials provided in examples 1 to 4 and comparative examples 1 and 2 were subjected to the performance test, and the test results are shown in table 1:
TABLE 1 tables of data on the properties of rubber materials provided in examples and comparative examples
As can be seen from Table 1, the tensile strength of the rubber material provided in examples 1 to 4 of the present invention is 19.1MPa, the elongation at break is 421%, the Shore A hardness is 63, and the permanent deformation at break is 28.1%;
as can be seen from Table 1, the rubber materials provided by the examples of the present invention have significantly higher tensile strength and tensile elongation.
FIG. 2 is a graph showing the tensile hysteresis curves at 200% elongation of rubber materials provided in example 1 of the present invention and comparative example 1, wherein curve a is the tensile hysteresis curve of comparative example 1 and curve b is the tensile hysteresis curve of example 1, and as shown in FIG. 2, the hysteresis energy (365X 10) of the rubber material provided in example 1 is shown4J/m2) Is comparative example 1 (120X 10)4J/m2) 3 times higher, showing good energy dissipation capacity and toughness.
Claims (2)
1. The preparation method of the rubber material is characterized by comprising the following steps of:
step 1, mixing methacrylic acid and montmorillonite modified by a cationic surfactant to prepare slurry;
step 2, mixing the plasticated rubber and the sizing agent, then adding a vulcanizing agent and an anti-aging agent for mixing,
obtaining mixed rubber;
step 3, vulcanizing the rubber compound to obtain a rubber material;
the components in the steps 1 and 2 are mixed according to the following mass portions:
100 parts of rubber, 10-30 parts of methacrylic acid, 5-15 parts of montmorillonite modified by a cationic surfactant, 1-6 parts of a vulcanizing agent and 1-3 parts of an anti-aging agent;
the rubber in the step 2 is one or more of nitrile rubber or hydrogenated nitrile rubber with the acrylonitrile mass content of 18-45%;
mixing the plasticated rubber with the slurry in the step 2 comprises the following steps:
mixing the plasticated rubber with the slurry at 90-110 ℃ for not less than 5 min;
before the vulcanizing agent and the anti-aging agent are added and mixed in the step 2, the method further comprises the following steps:
cooling the mixed nitrile rubber and the slurry to below 40 ℃;
and (3) vulcanizing at the temperature of 140-170 ℃ and under the pressure of 5-15 MPa.
2. The method for producing a rubber material according to claim 1, characterized in that:
the vulcanizing agent in the step 2 is one or two combinations of dicumyl peroxide and 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane;
the anti-aging agent in the step 2 is one or a combination of more than one of amine and phenol anti-aging agents.
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