CN113754944B - High-performance multi-network-structure elastomer and preparation method thereof - Google Patents
High-performance multi-network-structure elastomer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of elastomers, in particular to a high-performance elastomer with a multi-network structure and a preparation method thereof, wherein ethylene acrylate rubber (AEM) is used as a base material, the ethylene acrylate rubber is composed of ethylene, methyl acrylate and vulcanization points, and the ethylene acrylate rubber uses hexamethylene diamine carbamate (Diak No.1, amines) as a vulcanization crosslinking agent; the used vulcanization crosslinking agent is an amine vulcanizing agent, and amino and carboxyl react to form amido bond; the method is simple and easy to operate to prepare the high-performance elastomer, and completely has the prospect of industrial application and popularization.
Description
Technical Field
The invention relates to the technical field of elastomers, in particular to a high-performance multi-network-structure elastomer and a preparation method thereof.
Background
The rubber material is an important high polymer material and is widely applied to industry, agriculture and daily life, such as tires, sealing parts, shock absorbing parts and the like. Because the modulus and the strength of the pure rubber are lower, the filler is required to be added to reinforce the rubber in actual use. Carbon black, white carbon black, montmorillonite and the like are used as common fillers for rubber reinforcement, and in recent years, new nano reinforcing fillers such as graphene, carbon nanotubes and the like are also used for rubber reinforcement. The filler can effectively improve the modulus and strength of the rubber, so that the rubber meets the mechanical property requirements of actual use. However, the use of conventional fillers reduces the adhesive properties of the rubber material, such as the adhesive modulus and the loss factor.
After the sacrificial bonds (such as coordination bonds, ionic bonds, hydrogen bonds and the like) are subjected to external force, energy is dissipated by breaking the sacrificial bonds to ensure the integrity of the covalent network. Therefore, in recent years, research and application have been widely conducted in the fields of self-repairing rubbers, shape memory rubbers, and high damping materials.
Disclosure of Invention
In order to solve the problems, the invention provides a simple and easy-to-operate method for preparing a high-performance elastomer, and the high-performance elastomer with a multi-network structure and the preparation method thereof have the prospect of industrial application and popularization.
The technical scheme adopted by the invention is as follows: a high-performance multi-network structure elastomer uses ethylene/Acrylic Elastomer (AEM) as a base material, the ethylene acrylate rubber is composed of ethylene, methyl acrylate and a vulcanization point, and the ethylene acrylate rubber uses hexamethylene diamine carbamate (Diak No.1, amine) as a vulcanization crosslinking agent.
In a further improvement of the above scheme, the used vulcanization crosslinking agent is an amine type vulcanizing agent, and the amino group and the carboxyl group react to form an amide bond (crosslinking point).
A method for preparing a high-performance elastomer with a multi-network structure,
the method comprises the following steps:
step S1, firstly, mixing AEM rubber and magnesium oxide (MgO) in an internal mixer for 20min, then cooling to room temperature and discharging;
s2, placing the mixed rubber into a roll of an open rubber mixing mill, then respectively adding auxiliary agents such as N, N' -di-o-tolylguanidine (DOTG), stearic acid, polyoxyethylene octadecyl ether phosphate, diak No.1 (the auxiliary agents are added one by one in sequence), mixing for 8 minutes, performing triangular wrapping three times in the mixing period, and cutting 3/4 cutter three times; finally, the rubber compound is taken out of the roller for the last time to prepare a sheet sample with the thickness of about 0.4 cm;
and S3, sampling 65-70 g/piece of the mixed rubber, putting the mixed rubber into a mold, and putting the mold into a flat vulcanizing machine to vulcanize for 30 minutes at 170 ℃ to obtain the high-performance multi-network-structure elastomer.
In a further improvement of the above solution, in step S1, the AEM rubber used is composed of ethylene, acrylate and a vulcanization site containing a carboxyl group.
In a further improvement of the above scheme, in the step S1, the mixing temperature of the AEM rubber and magnesium oxide (MgO) is 120 +/-5 ℃; the MgO is directly put into and mixed at one time.
The scheme is further improved in that in the step S2, the temperature of the open rubber mixing mill is lower than 60 ℃; the weight ratio of the AEM rubber, the N, N' -di-o-tolylguanidine and the polyoxyethylene octadecyl ether phosphate is (100).
The scheme is further improved in that the dosage mass ratio of the magnesium oxide (MgO) to the AEM rubber is 5-10; the weight ratio of the stearic acid to the MgO is 3.
In a further improvement of the scheme, the MgO and the acidic functional group in the AEM generate Mg < 2+ > to form a metal-ligand structure with an N atom in an amine vulcanizing agent.
In a further improvement of the above, the MgO forms Mg2+ with the acidic functional groups in the AEM.
The further improvement of the scheme is that after the MgO is added, besides a common covalent structure, a multiple network structure such as an ion structure, a coordination structure and the like is formed in the AEM matrix.
The invention has the beneficial effects that:
the preparation method is simple to operate and suitable for large-scale production; the preparation method comprises the steps of mixing magnesium oxide with AEM rubber to perform acid-base reaction to generate metal Mg ions, wherein Mg < 2+ > and N atoms in amine vulcanizing agents can form a metal-coordination structure, and the metal-coordination structure is preferentially broken and dissipates energy under the action of external force to protect the covalent structure of a rubber matrix, so that the rubber matrix has better damping performance; the metal Mg < 2+ > can form ionic bonds with groups such as carboxylic acid and the like, and the rubber matrix has higher elastic modulus (namely rigidity) and tensile strength due to stronger ionic bonds.
The high-performance rubber provided by the invention can form two special chemical bonds of coordination bonds and ionic bonds in a rubber matrix by the produced metal ions through the reaction of the special functional group of the AEM rubber and the metal oxide. The two chemical bonds show completely different characteristics from covalent bonds, so that on one hand, the damping performance of the rubber is improved; on the other hand, the mechanical property and the rigidity of the rubber are improved.
In the present invention, the elastomer matrix is an ethylene-acrylate rubber (AEM) with hexamethylenediamine carbamate as the vulcanization cross-linking agent. Because the AEM rubber contains acidic functional groups, magnesium ions can be formed after magnesium oxide is added, mg < 2+ > not only can form a metal-coordination structure with an amine vulcanizing agent to improve the tensile strength and toughness of the elastomer, but also can form metal ion aggregation to improve the mechanical property and modulus of the elastomer; the invention utilizes magnesium oxide to construct two structures of coordination and ions in AEM rubber, and invents a simple and easy-to-operate method to prepare high-performance elastomer, thereby completely having the prospect of industrial application and popularization.
Description of the drawings:
FIG. 1 is the mechanical properties of different metal oxide filled AEM rubbers;
FIG. 2 is the storage modulus of AEM rubber with different metal oxides added
FIG. 3 is a graph of loss factor for AEM rubber with different metal oxides added;
FIG. 4 is a thermogravimetric plot of zinc oxide filled AEM rubber;
FIG. 5 is a thermogravimetric plot of magnesia filled AEM rubber.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
A high-performance multi-network structure elastomer uses ethylene/Acrylic Elastomer (AEM) as a base material, wherein the ethylene acrylate rubber is composed of ethylene, methyl acrylate and vulcanization points, and hexamethylene diamine carbamate (Diak No.1, amine) is used as a vulcanization crosslinking agent. The cross-linking agent used in vulcanization is an amine-type vulcanizing agent, and the amino group and the carboxyl group react to form an amide bond (cross-linking point).
The elastomer matrix is an ethylene-acrylate rubber (AEM) with hexamethylene diamine carbamate as the vulcanization crosslinking agent. Because the AEM rubber contains acidic functional groups, magnesium ions can be formed after magnesium oxide is added, mg < 2+ > not only can form a metal-coordination structure with an amine vulcanizing agent to improve the tensile strength and toughness of the elastomer, but also can form metal ion aggregation to improve the mechanical property and modulus of the elastomer.
A method for preparing a high-performance elastomer with a multi-network structure,
the method comprises the following steps:
step S1, firstly, mixing AEM rubber and magnesium oxide (MgO) in an internal mixer for 20min, then cooling to room temperature and discharging;
step S2, placing the mixed rubber on a roll of an open rubber mixing mill, then respectively adding auxiliary agents (the auxiliary agents are sequentially added one by one) such as N, N' -di-o-tolylguanidine (DOTG), stearic acid, polyoxyethylene octadecyl ether phosphate ester, diak No.1, and the like, mixing for 8 minutes, triangular wrapping three times during the mixing, and cutting for 3/4 times; finally, the rubber compound is taken out of the roller for the last time to prepare a sheet sample with the thickness of about 0.4 cm;
and S3, sampling 65-70g of the rubber compound per sheet, placing the rubber compound in a mold, and placing the mold in a flat vulcanizing machine for vulcanizing for 30 minutes at 170 ℃ to obtain the high-performance multi-network-structure elastomer.
In step S1, the AEM rubber used is composed of ethylene, acrylic ester and a vulcanization site containing a carboxyl group.
In the step S1, the mixing temperature of the AEM rubber and the magnesium oxide (MgO) is 120 +/-5 ℃; the MgO feeding and mixing method is one-time direct feeding and mixing.
In the step S2, the temperature of the open rubber mixing mill is lower than 60 ℃; the weight ratio of the AEM rubber, the N, N' -di-o-tolylguanidine and the polyoxyethylene octadecyl ether phosphate is (100).
The mass ratio of the magnesium oxide (MgO) to the AEM rubber is 5-10; the weight ratio of the stearic acid to the MgO is 3.
Mg < 2+ > is generated by MgO and an acidic functional group in AEM and forms a metal-ligand structure with N atoms in an amine vulcanizing agent; the mechanical property of the elastomer is improved and the toughness is improved.
Mg < 2+ > is generated by acidic functional groups in MgO and AEM, and metal magnesium ions cause the aggregation of ion clusters due to stronger ion interaction force, so that the mechanical property and the dynamic modulus of the elastomer are effectively improved.
After MgO is added, besides a common covalent structure, multiple network structures such as an ion structure, a coordination structure and the like are formed in an AEM matrix; the mechanical property and dynamic modulus of the AEM rubber are obviously improved, and the toughness of the AEM rubber is effectively improved.
In the present invention, the elastomer matrix is an ethylene-acrylate rubber (AEM) with hexamethylenediamine carbamate as the vulcanization crosslinking agent. Because the AEM rubber contains acidic functional groups, magnesium ions can be formed after magnesium oxide is added, mg < 2+ > not only can form a metal-coordination structure with an amine vulcanizing agent to improve the tensile strength and toughness of the elastomer, but also can form metal ion aggregation to improve the mechanical property and modulus of the elastomer; the invention utilizes the magnesium oxide to construct two structures of coordination and ions in AEM rubber, invents a simple and easy-to-operate method to prepare the high-performance elastomer, and has completely industrialized application and popularization prospects.
The preparation method is simple to operate and suitable for large-scale production; the preparation method comprises the steps of mixing magnesium oxide with AEM rubber to perform acid-base reaction to generate metal Mg ions, wherein Mg < 2+ > and N atoms in amine vulcanizing agents can form a metal-coordination structure, and the metal-coordination structure is preferentially broken and dissipates energy under the action of external force to protect the covalent structure of a rubber matrix, so that the rubber matrix has better damping performance; the metal Mg < 2+ > can form ionic bonds with groups such as carboxylic acid and the like, and the rubber matrix has higher elastic modulus (namely rigidity) and tensile strength due to the stronger ionic bonds.
Example 1
A preparation method (blank sample) of high-performance multi-network structure rubber comprises the following steps:
(1) Firstly weighing 100 parts by weight of ethylene-acrylate rubber, placing the ethylene-acrylate rubber in an internal mixer to be stirred for 33min, wherein the stirring temperature is 120 +/-5 ℃, then discharging, and cooling to room temperature;
(2) Respectively weighing 4 parts by weight, 1.5 parts by weight and 1.5 parts by weight of N, N' -di-o-tolylguanidine (DOTG), stearic acid, polyoxyethylene octadecyl ether phosphate and hexamethylene diamine carbamate (Diak No. 1);
(3) Placing AEM on a roll of an open mill, cooling with cooling water, adding the four additives respectively, cutting for three times by 3/4 in the mixing process, packaging with a triangular bag for three times to uniformly disperse the additives in the rubber material, taking out the sheet, placing the sheet in a drying place, and controlling the temperature of the roll of the open mill to be lower than 60 ℃;
(4) Vulcanizing the AEM rubber compound in a flat vulcanizing machine, wherein the vulcanization temperature is 170 ℃, the vulcanization time is 30min, and the standby performance of a vulcanized test piece is tested;
example 2
A preparation method of high-performance multi-network structure rubber (zinc oxide control sample) comprises the following steps:
(1) Weighing 100 parts by weight of ethylene-acrylate rubber, placing the ethylene-acrylate rubber in an internal mixer, stirring for 3min, then placing 5 parts by weight of zinc oxide in the internal mixer, mixing the ethylene-acrylate rubber and the zinc oxide at the mixing temperature of 120 +/-5 ℃ for 30min, then discharging, and cooling to room temperature;
(2) Respectively weighing 4 parts, 1.5 parts and 1.5 parts of N, N' -di-o-tolylguanidine (DOTG), stearic acid, polyoxyethylene octadecyl ether phosphate and hexamethylene diamine carbamate (Diak No. 1);
(3) Placing AEMZnO rubber compound into a roll of an open mill, cooling with cooling water, adding the four additives respectively, cutting 3/4 of the roll three times in the mixing process, packaging in a triangular manner three times to uniformly disperse the additives in rubber material, taking out the rubber compound and placing the rubber compound in a drying place, and controlling the temperature of the roll of the open mill to be lower than 60 ℃;
(4) And vulcanizing the AEM/ZnO rubber compound in a flat vulcanizing machine, wherein the vulcanizing temperature is 170 ℃, the vulcanizing time is 30min, and the standby performance of a vulcanized test piece is tested.
Example 3
A preparation method of high-performance multi-network structure rubber comprises the following steps:
(1) Weighing 100 parts by weight of ethylene-acrylate rubber, placing the ethylene-acrylate rubber in an internal mixer, stirring for 3min, then placing 5 parts by weight of zinc oxide in the internal mixer, mixing the ethylene-acrylate rubber and the zinc oxide at the mixing temperature of 120 +/-5 ℃ for 30min, then discharging, and cooling to room temperature;
(2) Respectively weighing 4 parts, 1.5 parts and 1.5 parts of N, N' -di-o-tolylguanidine (DOTG), stearic acid, polyoxyethylene octadecyl ether phosphate and hexamethylene diamine carbamate (Diak No. 1);
(3) Placing AEMZnO rubber compound into a roll of an open mill, cooling with cooling water, adding the four additives respectively, cutting 3/4 of the roll three times in the mixing process, packaging in a triangular manner three times to uniformly disperse the additives in rubber material, taking out the rubber compound and placing the rubber compound in a drying place, and controlling the temperature of the roll of the open mill to be lower than 60 ℃;
(4) And vulcanizing the AEM/ZnO rubber compound in a flat vulcanizing machine, wherein the vulcanizing temperature is 170 ℃, the vulcanizing time is 30min, and the standby performance of a vulcanized test piece is tested.
Example 4
The specific preparation method is substantially the same as that of example 3, except that: the mass fraction of the magnesium oxide is 10.
Example 5
The specific preparation method is substantially the same as that of example 3, except that: the mass fraction of magnesium oxide is 15.
Performance testing of the high performance multi-network AEM rubber prepared in the above examples is shown below
Referring to fig. 1, the mechanical properties of different metal oxide filled AEM rubbers;
referring to fig. 2, the storage modulus of AEM rubber with different metal oxides added;
referring to fig. 3, the loss factor of AEM rubber with different metal oxides added;
referring to fig. 4-5, thermogravimetric curves for zinc oxide and magnesium oxide filled AEM rubber;
the above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. A preparation method of a high-performance elastomer with a multi-network structure is characterized by comprising the following steps:
a high-performance multi-network elastomer using ethylene/Acrylic Elastomer (AEM) as a base material, the ethylene acrylate rubber being composed of ethylene, methyl acrylate and a vulcanization site, the ethylene acrylate rubber using hexamethylenediamine carbamate (Diak No.1, amine) as a vulcanization crosslinking agent;
the vulcanization crosslinking agent is an amine vulcanizing agent, and amino and carboxyl react to form amido bond;
the preparation method comprises the following steps:
step S1, firstly, mixing AEM rubber and magnesium oxide (MgO) in an internal mixer for 20min, then cooling to room temperature and discharging;
s2, placing the mixed rubber on a roll of an open rubber mixing mill, then adding N, N' -di-o-tolylguanidine (DOTG), stearic acid, polyoxyethylene octadecyl ether phosphate and a Diak No.1 auxiliary agent one by one in sequence, mixing for 8 minutes, triangular wrapping three times during the mixing, and cutting 3/4 cutter three times; finally, the rubber compound is taken out of the roller for the last time to prepare a sheet sample with the thickness of about 0.4 cm;
s3, sampling 65-70 g/piece of mixed rubber, placing the mixed rubber in a mold, and placing the mold in a flat vulcanizing machine at 170 DEG 0 C, vulcanizing for 30 minutes to obtain a high-performance multi-network-structure elastomer;
the mass ratio of the magnesium oxide (MgO) to the AEM rubber is 5-10; the weight ratio of the stearic acid to the MgO is 3.
2. The method for preparing the high-performance multi-network-structure elastomer according to claim 1, wherein: in step S1, the AEM rubber used is composed of ethylene, acrylic acid ester, and a vulcanization site containing a carboxyl group.
3. The method for preparing the high-performance multi-network-structure elastomer according to claim 2, wherein: in the step S1, the mixing temperature of AEM rubber and magnesium oxide (MgO) is 120 +/-5 0 C; the MgO feeding and mixing method is one-time direct feeding and mixing.
4. The method for preparing the high-performance multi-network-structure elastomer according to claim 1, wherein: in the step S2, the temperature of the open rubber mixing mill is lower than 60 ℃; the weight ratio of the AEM rubber, the N, N' -di-o-tolylguanidine and the polyoxyethylene octadecyl ether phosphate is 100.
5. The method for preparing the high-performance multi-network-structure elastomer according to claim 1, wherein: the MgO and the acid functional group in the AEM generate Mg < 2+ > to form a metal-ligand structure with the N atom in the amine vulcanizing agent.
6. The method for preparing the high-performance multi-network-structure elastomer according to claim 1, wherein: the MgO reacts with the acidic functional groups in the AEM to form Mg2+.
7. The method for preparing the high-performance multi-network-structure elastomer according to claim 1, wherein: after the addition of MgO, besides the common covalent structure, a multiple network structure of an ionic structure and a coordination structure is formed in the AEM matrix.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3910866A (en) * | 1973-09-17 | 1975-10-07 | Roger E Morris | Acrylate rubber vulcanizable compositions |
| JP2010090351A (en) * | 2008-10-11 | 2010-04-22 | Nok Corp | Acrylic rubber composition and seal parts vulcanized and molded using same |
| CN105176101A (en) * | 2015-08-17 | 2015-12-23 | 合肥市再德高分子材料有限公司 | High-performance modified acrylate rubber material and preparation method thereof |
| CN106336564A (en) * | 2016-08-29 | 2017-01-18 | 樊之雄 | Low-temperature-resistant and corrosion-resistant rubber tube and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8921460B2 (en) * | 2011-06-21 | 2014-12-30 | E. I. Du Pont De Nemours And Company | Heat-stabilized acrylate elastomer composition and process for its production |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3910866A (en) * | 1973-09-17 | 1975-10-07 | Roger E Morris | Acrylate rubber vulcanizable compositions |
| JP2010090351A (en) * | 2008-10-11 | 2010-04-22 | Nok Corp | Acrylic rubber composition and seal parts vulcanized and molded using same |
| CN105176101A (en) * | 2015-08-17 | 2015-12-23 | 合肥市再德高分子材料有限公司 | High-performance modified acrylate rubber material and preparation method thereof |
| CN106336564A (en) * | 2016-08-29 | 2017-01-18 | 樊之雄 | Low-temperature-resistant and corrosion-resistant rubber tube and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 硫化时间对AEM性能的影响;张洪振等;《特种橡胶制品》;20110615;34-37 * |
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