CN115651322A - Sulfur-free anti-overheating water sealing ring - Google Patents
Sulfur-free anti-overheating water sealing ring Download PDFInfo
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- CN115651322A CN115651322A CN202211388500.8A CN202211388500A CN115651322A CN 115651322 A CN115651322 A CN 115651322A CN 202211388500 A CN202211388500 A CN 202211388500A CN 115651322 A CN115651322 A CN 115651322A
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Abstract
The invention relates to a sulfur-free anti-overheating water seal ring, which mainly solves the problems that the existing seal ring is easy to age in hot water and poor in anti-overheating steam performance, and shows lower compression deformation and thermal performance by adding a self-made anti-aging agent HVA-2@ MB, wherein the sulfur-free anti-overheating water seal ring comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer; 35 to 60 parts of filler; 5 to 15 portions of peroxide and accelerator; 5 to 15 parts of plasticizer; 2 to 5 parts of an antioxidant; 2 to 4 parts of an anti-aging agent; the technical scheme of 2 to 5 parts of the coupling agent better solves the technical problem and can be used for producing the sealing ring.
Description
Technical Field
The invention belongs to the field of sealing ring materials, and particularly relates to a sulfur-free superheated water-resistant sealing ring.
Background
In the production process of the sealing ring, the compression permanent deformation performance of the rubber material directly influences the service life and the sealing performance of the sealing ring, and the requirement on the compression permanent deformation of rubber is more severe in the sealing ring for the hot water pipe due to the high temperature of the environment. The sealing ring applied to the high-pressure hot water pipe not only requires the mechanical property of the sizing material, but also puts new requirements on the aging resistance and the hot water resistance of the sizing material.
The ethylene propylene diene monomer is polymerized by adding a small amount of non-conjugated diene into ethylene and propylene monomers, so that the main chain of the ethylene propylene diene monomer has no unsaturated double bonds, and the ethylene propylene diene monomer has the advantages of heat resistance, ozone resistance, weather resistance, good processability and low compression set, and is a preferred material for a non-polar sealing ring. The ethylene propylene diene monomer is nonpolar rubber, has excellent hot water resistance, and the cross-linking bond between the rubber is mainly C-S-C bond when sulfur vulcanization is adopted, and has longer bond length, poorer heat resistance and poorer compression set compared with the C-C bond produced by peroxide vulcanization. Therefore, the sealing ring prepared by vulcanizing the peroxide of the ethylene propylene rubber is suitable for high-pressure hot water environment.
Disclosure of Invention
The invention aims to solve the technical problem that the prior art has poor superheated water resistance, and provides a novel sealing ring formula, which has the characteristics of low compression permanent deformation, superheated water resistance, no odor and no odor.
The second technical problem to be solved by the present invention is to provide a manufacturing method of a seal ring.
To solve one of the above technical problems, the technical solution of the present invention is as follows.
The sulfur-free anti-overheating water sealing ring comprises the following components in parts by weight:
100 parts of ethylene propylene diene monomer; 35 to 60 parts of carbon black; 2 to 10 parts of zinc oxide; 1 to 5 parts of peroxide vulcanizing agent; 5 to 15 parts of a vulcanization accelerator; 5 to 15 parts of paraffin oil; anti-aging agent HVA-2@ MB,2 to 4 parts; 2-5 parts of a silane coupling agent.
The preparation method of the anti-aging agent HVA-2@ MB comprises the following steps:
2-5g of HVA-2 and 2-5g of MB were added to 150mL of tetrahydrofuran and, after complete dissolution by sonication, the solution was transferred to a three-necked flask equipped with a reflux condenser and a magnetic stirrer. Under the protection of N2 atmosphere, the reaction solution is heated to 50-80 ℃, and then 0.1-1 g of catalyst triethylamine is injected by an injector. After 24 hours the reaction was complete and the solvent was removed from the reaction mixture by rotary evaporation to give the crude product as a solid. The solid crude product was washed with methanol and then centrifuged to obtain a purified product, which was then dried in a vacuum oven for 24 hours.
To solve the second technical problem, the technical solution of the present invention is as follows:
a method for producing a gasket, comprising processing the composition according to any one of the above-mentioned aspects of the present invention into a gasket by a platen molding method or an injection molding method.
In the above technical solution, when the extrusion pressing plate forming method is adopted, the following steps may be optionally included: the method comprises the following steps:
(1) Weighing the raw materials according to the weight, mixing by using an internal mixer, wherein the initial temperature of the internal mixer is 70-80 ℃, the rotating speed of the internal mixer is 30-40rad/min, then adding various ingredients according to the weight ratio of 1.1-1.5, and the adding order of the ingredients is as follows: zinc oxide, stearic acid, zinc acrylate, an anti-aging agent, peroxide, a silane coupling agent and finally adding carbon black. And (3) mixing and uniformly mixing by using an internal mixer.
(2) Placing the rubber compound in a mold, and vulcanizing by using a flat vulcanizing instrument; and preheating a flat vulcanizing instrument to 110 to 150 ℃, putting the mold into the flat vulcanizing instrument, prepressing for 5 to 10min, then exhausting, and vulcanizing for 15 to 20min to obtain the sealing ring.
The invention has the beneficial effects that:
HVA-2 is a co-curing agent in a peroxide curing system, and the antioxidant MB is used as an antioxidant to inhibit the formation of cross-linked bonds in the peroxide curing system, and has great influence on the permanent compression deformation performance after the cross-linked density is reduced. When HVA-2 was grafted with antioxidant MB, the reactive thiol groups in MB were already consumed by HVA-2@ MB, which reduced the reaction of MB with alkoxy radicals. Therefore, the auxiliary crosslinking effect of HVA-2@ MB compensates for the scavenging effect of MB on alkoxy free radicals, and finally, HVA-2@ MB/EPDM can increase the crosslinking density of the rubber. In addition, nitrogen and oxygen atoms existing in HVA-2@ MB can form hydrogen bonds, so that the interaction between rubber molecular chains is enhanced, and the mechanical property of the rubber is improved.
Mechanical Property test
The elongation at break is tested by a universal tensile testing machine according to the GB/T528-2009 standard, the tested dumbbell-shaped sample is prepared by a GB/T2941-2006 dumbbell-shaped sample cutter, each experimental sample bar is tested for 5 times at the temperature of 25 ℃ and the tensile speed of 50 mm/min, and the average value of the final results is taken.
Shore a hardness test
The hardness of the test sample is measured by using a Shore A hardness tester, and 5 points are selected from the sample to perform the test and take an average value.
Tear Strength test
The tearing strength is tested by a GB/T529-2008 standard through a universal tensile testing machine, a right-angle sample to be tested is prepared by a GB/T529-2008 right-angle tearing cutter, each experimental sample bar is tested for 5 times at 25 ℃ under the condition that the tensile speed is 50 mm/min, and the average value of the final results is taken.
Compression set test
The compression set is tested by a compression deflection tester according to the GB/T1687-1993 standard, and the tested cylindrical sample meets the size requirement of a GB 5723 sample, the diameter is 17.8 +/-0.15 mm, and the height is 25 +/-0.25 mm. The samples were subjected to compression set tests at 125 ℃ for 24h with a compression ratio of 15% as specified in GB 2491.
Hot water resistance test
The hot water resistance is determined according to ISO 9361:2004 test Standard, cylinder test specimens are immersed in superheated water in a kettle at 110 ℃ for 500 hours to test the compression set.
Detailed Description
Example 1
1. Ethylene propylene rubber formula
The rubber formula comprises the following components in parts by weight:
100 parts of ethylene propylene rubber;
40 parts of carbon black;
2 parts of stearic acid;
5 parts of zinc oxide;
3 parts of BIBP;
2 parts of TAIC;
PDM,2 parts;
6 parts of paraffin oil;
anti-aging agent HVA-2@ MB,1.5 parts.
2. Production of ethylene propylene rubber
The method comprises the following steps: weighing raw materials according to weight, mixing by using an internal mixer, wherein the initial temperature of the internal mixer is 75 ℃, the rotating speed is 35rad/min, firstly adding ethylene propylene rubber, and then adding various ingredients according to the charging sequence of zinc oxide, stearic acid, zinc oxide, an anti-aging agent, peroxide, paraffin oil and carbon black. And (3) mixing and uniformly mixing by using an internal mixer.
Step two: placing the rubber compound in a mold, and vulcanizing by using a flat vulcanizing instrument; preheating a flat vulcanizing instrument to 140 ℃, putting the die into the flat vulcanizing instrument, prepressing for 5min, exhausting, and vulcanizing for 15min to obtain the rubber material.
Through tests, the tensile strength of the rubber is 10.4 MPa, the hardness is 54 Shore A, the compression set is 16%, the tear strength is 21.6KN/m, the compression set is 16.8%, and the compression set is 61.5% after being aged in hot water at 110 ℃ for 500 h.
For comparison, the properties of the rubber and the vulcanization mode are shown in Table 1.
Example 2
1. Ethylene propylene rubber formula
The rubber formula comprises the following components in parts by weight:
100 parts of ethylene propylene rubber;
40 parts of carbon black;
2 parts of stearic acid;
5 parts of zinc oxide;
3 parts of DCP;
2 parts of TAIC;
PDM,2 parts;
paraffin oil, 6 parts;
1.5 parts of anti-aging agent RD;
1.5 parts of anti-aging agent MB.
2. Production of ethylene-propylene rubber
The method comprises the following steps: weighing raw materials according to weight, mixing by using an internal mixer, wherein the initial temperature of the internal mixer is 75 ℃, the rotating speed is 35rad/min, firstly adding ethylene propylene rubber, and then adding various ingredients according to the charging sequence of zinc oxide, stearic acid, zinc oxide, an anti-aging agent, peroxide, paraffin oil and carbon black. And (3) mixing and uniformly mixing by using an internal mixer.
Step two: placing the rubber compound in a mold, and vulcanizing by using a flat vulcanizing instrument; preheating a flat vulcanizing instrument to 140 ℃, putting the die into the flat vulcanizing instrument, prepressing for 5min, exhausting, and vulcanizing for 15min to obtain the rubber material.
Through tests, the tensile strength of the rubber is 8.3 MPa, the hardness is 55 Shore A, the tear strength is 15.1 KN/m, the compression set is 27.6%, and the compression set is 69.3% after being aged by hot water at 110 ℃ for 500 h.
For comparison, the properties of the rubber and the vulcanization mode are shown in Table 1.
Example 3
1. Ethylene propylene rubber formula
100 parts of ethylene propylene rubber;
40 parts of carbon black;
2 parts of stearic acid;
5 parts of zinc oxide;
3 parts of BIBP;
0.5 part of sublimed sulfur;
PDM,2 parts;
6 parts of paraffin oil;
anti-aging agent HVA-2@ MB,1.5 parts.
2. Production of ethylene propylene rubber
The method comprises the following steps: weighing raw materials according to weight, mixing by using an internal mixer, wherein the initial temperature of the internal mixer is 75 ℃, the rotating speed is 35rad/min, firstly adding ethylene propylene rubber, and then adding various ingredients according to the charging sequence of zinc oxide, stearic acid, zinc oxide, an anti-aging agent, sublimed sulfur, peroxide, paraffin oil and carbon black. And (3) mixing and uniformly mixing by using an internal mixer.
Step two: placing the rubber compound in a mold, and vulcanizing by using a flat vulcanizing instrument; preheating a flat vulcanizing instrument to 120 ℃, putting the die into the flat vulcanizing instrument, prepressing for 3min, exhausting, and vulcanizing for 12min to obtain the rubber material.
Through tests, the tensile strength of the rubber is 14.5 MPa, the hardness is 55 Shore A, the tear strength is 24.1 KN/m, the compression set is 29.2%, and the compression set after hot water aging at 110 ℃ for 500 hours is 77.5%.
For comparison, the properties of the rubber and the vulcanization mode are shown in Table 1.
Example 4
1. Ethylene propylene rubber formula
The rubber formula comprises the following components in parts by weight:
100 parts of ethylene propylene rubber;
40 parts of carbon black;
2 parts of stearic acid;
5 parts of zinc oxide;
3 parts of DCP;
0.5 part of sublimed sulfur;
PDM,2 parts;
6 parts of paraffin oil;
1.5 parts of an anti-aging agent RD;
1.5 parts of an anti-aging agent MB.
2. Production of ethylene-propylene rubber
The method comprises the following steps: weighing raw materials according to weight, mixing by using an internal mixer, wherein the initial temperature of the internal mixer is 75 ℃, the rotating speed is 35rad/min, firstly adding ethylene propylene rubber, and then adding various ingredients according to the charging sequence of zinc oxide, stearic acid, zinc oxide, an anti-aging agent, sublimed sulfur, peroxide, paraffin oil and carbon black. And (3) mixing and uniformly mixing by using an internal mixer.
Step two: placing the rubber compound in a mold, and vulcanizing by using a flat vulcanizing instrument; preheating a flat vulcanizing instrument to 120 ℃, putting the die into the flat vulcanizing instrument, prepressing for 3min, exhausting, and vulcanizing for 12min to obtain the rubber material.
Through tests, the tensile strength of the rubber is 13.7 MPa, the hardness is 56 Shore A, the tear strength is 26.2KN/m, the compression set is 34.1%, and the compression set is 79.4% after being aged by hot water at 110 ℃ for 500 h.
For comparison, the properties of the rubber and the vulcanization mode are shown in Table 1.
Comparative example
1. Ethylene propylene rubber formula
The rubber formula comprises the following components in parts by weight:
100 parts of ethylene propylene rubber;
40 parts of carbon black;
2 parts of stearic acid;
5 parts of zinc oxide;
2.5 parts of an accelerator M;
accelerator TT,1 part;
1.5 parts of accelerator BZ;
1.5 parts of sublimed sulfur;
6 parts of paraffin oil;
1.5 parts of an anti-aging agent RD;
1.5 parts of an anti-aging agent MB.
2. Production of ethylene-propylene rubber
The method comprises the following steps: weighing raw materials according to weight, mixing by using an internal mixer, wherein the initial temperature of the internal mixer is 75 ℃, the rotating speed is 35rad/min, firstly adding ethylene propylene rubber, and then adding various ingredients according to the charging sequence of zinc oxide, stearic acid, zinc oxide, an anti-aging agent, sublimed sulfur, paraffin oil and carbon black. And (3) mixing and uniformly mixing by using an internal mixer.
Step two: placing the rubber compound in a mold, and vulcanizing by using a flat vulcanizing instrument; preheating a flat vulcanizing instrument to 120 ℃, putting the die into the flat vulcanizing instrument, prepressing for 8min, exhausting, and vulcanizing for 10min to obtain the rubber material.
According to tests, the tensile strength of the rubber is 11.1MPa, the hardness is 58 Shore A, the tear strength is 23.2KN/m, the compression set is 40.6%, and the compression set after hot water aging at 110 ℃ for 500 hours is 86.7%.
For comparison, the properties of the rubber and the vulcanization mode are shown in Table 1.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
TABLE 1 summary of test properties for examples and comparative examples
| Example one | Example two | Example three | Example four | Comparative example | |
| Peroxide vulcanization | Is that | Is that | Is that | Is that | Whether or not |
| Sulphur vulcanization | Whether or not | Whether or not | Is that | Is that | Is that |
| Addition of HVA-2@ MB | Is that | Whether or not | Is that | Whether or not | Whether or not |
| Tensile strength/MPa | 10.4 | 8.3 | 14.5 | 13.7 | 11.1 |
| hardness/Shore A | 54 | 55 | 55 | 56 | 58 |
| Tear Strength/KN/m | 21.6 | 15.1 | 24.1 | 26.2 | 23.2 |
| Voltage transformer (125 ℃/24 h) | 16.8% | 27.6% | 29.2% | 34.1% | 40.6% |
| Permanent deformation of 500h-110 DEG C | 61.5% | 69.3% | 77.5% | 79.4% | 86.7% |
Claims (4)
1. The sulfur-free anti-overheating water sealing ring comprises the following components in parts by weight:
100 parts of ethylene propylene diene monomer; 35 to 60 parts of carbon black; 2 to 10 parts of zinc oxide; 1 to 5 parts of peroxide vulcanizing agent; 5 to 15 parts of a vulcanization accelerator; 5 to 15 parts of paraffin oil; 2 to 5 parts of a silane coupling agent; 2 to 5 portions of self-made anti-aging agent HVA-2@ MB.
2. The self-made antioxidant HVA-2@ MB according to claim 1, which is synthesized by adding 2-5g HVA-2 and 2-5g MB to 150mL tetrahydrofuran, after completely dissolving by sonication, transferring the solution to a three-necked flask equipped with a reflux condenser and a magnetic stirrer under N 2 The reaction solution was heated to 50-80 ℃ under the protection of atmosphere, then 0.1-1 g of catalyst triethylamine was injected with a syringe, the reaction was completed after 24 hours, the solvent in the reaction mixture was removed by rotary evaporation to obtain a solid crude product, which was washed with methanol and then centrifuged to obtain a purified product, which was then dried in a vacuum oven for 24 hours.
3. The sulfur-free heat-resistant water seal ring according to claim 1, wherein said peroxide curing agent is one or more selected from the group consisting of dicumyl peroxide, m-phenylene bismaleimide, triallyl isocyanurate, 1, 4-bis-t-butylperoxyisopropyl benzene.
4. The preparation method of the sulfur-free anti-overheating water sealing ring is characterized by comprising the following steps:
(1) Weighing raw materials according to weight, mixing by using an internal mixer, wherein the initial temperature of the internal mixer is 70 to 80 ℃, the rotating speed of the internal mixer is 30 to 40rad/min, then adding various ingredients according to the weight ratio of 1.1 to 1.5, and the adding order of the ingredients is as follows: zinc oxide, stearic acid, zinc acrylate, an anti-aging agent, peroxide and a silane coupling agent, and finally adding carbon black, and mixing and uniformly mixing by using an internal mixer; (2) Placing the rubber compound in a mold, and vulcanizing by using a flat vulcanizing instrument; and (3) preheating a flat vulcanizing instrument to 110-150 ℃, putting the mold into the flat vulcanizing instrument, prepressing for 5-10min, exhausting, and vulcanizing for 15-20min to obtain the sealing ring.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211388500.8A CN115651322A (en) | 2022-11-08 | 2022-11-08 | Sulfur-free anti-overheating water sealing ring |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211388500.8A CN115651322A (en) | 2022-11-08 | 2022-11-08 | Sulfur-free anti-overheating water sealing ring |
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| CN115651322A true CN115651322A (en) | 2023-01-31 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875905A (en) * | 2012-09-27 | 2013-01-16 | 青岛开世密封工业有限公司 | Low-pressure-variation ethylene-propylene rubber mixed compound and mixing method |
| CN106117840A (en) * | 2016-08-02 | 2016-11-16 | 天津包博特密封科技有限公司 | A kind of high impact resistance, shear-stable EPDM glue material |
| CN109401085A (en) * | 2018-11-28 | 2019-03-01 | 陕西秦垒建设集团有限公司 | A kind of EPT rubber packing item and preparation method thereof |
| CN110698774A (en) * | 2019-11-22 | 2020-01-17 | 广东贝洛新材料科技有限公司 | Ethylene propylene diene monomer rubber material capable of resisting heat at 150 ℃ and low pressure change, sealing ring and preparation method |
-
2022
- 2022-11-08 CN CN202211388500.8A patent/CN115651322A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875905A (en) * | 2012-09-27 | 2013-01-16 | 青岛开世密封工业有限公司 | Low-pressure-variation ethylene-propylene rubber mixed compound and mixing method |
| CN106117840A (en) * | 2016-08-02 | 2016-11-16 | 天津包博特密封科技有限公司 | A kind of high impact resistance, shear-stable EPDM glue material |
| CN109401085A (en) * | 2018-11-28 | 2019-03-01 | 陕西秦垒建设集团有限公司 | A kind of EPT rubber packing item and preparation method thereof |
| CN110698774A (en) * | 2019-11-22 | 2020-01-17 | 广东贝洛新材料科技有限公司 | Ethylene propylene diene monomer rubber material capable of resisting heat at 150 ℃ and low pressure change, sealing ring and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| QINGKUN LIU: "Synthesis and antioxidation behavior in EPDM of novel macromolecular antioxidants with crosslinking and antioxidation effects", 《POLYMER DEGRADATION AND STABILITY》, pages 110155 * |
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