CN110628163A - Low-compression permanent deformation ethylene propylene diene monomer sealing material and preparation method thereof - Google Patents
Low-compression permanent deformation ethylene propylene diene monomer sealing material and preparation method thereof Download PDFInfo
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- CN110628163A CN110628163A CN201910736643.5A CN201910736643A CN110628163A CN 110628163 A CN110628163 A CN 110628163A CN 201910736643 A CN201910736643 A CN 201910736643A CN 110628163 A CN110628163 A CN 110628163A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/04—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to rubbers
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Abstract
The invention relates to ethylene propylene diene monomer rubber, and discloses an ethylene propylene diene monomer rubber sealing material with low compression set and a preparation method thereof, wherein the ethylene propylene diene monomer rubber is obtained by mixing and refining 100 parts by mass of raw materials, 70-80 parts by mass of the ethylene propylene diene monomer rubber is maleic anhydride grafted ethylene propylene diene monomer rubber, 15 ~ parts by mass of a filler comprises freeze-thaw powder, the freeze-thaw powder accounts for more than 33 wt% of the filler, the particle size of the freeze-thaw powder is 400-600nm, the preparation method of the freeze-thaw powder comprises the steps of mixing uncalcined shell powder with 387 (~ -14 ℃) leachate at the mass ratio of 0.2.2 0.4:1, soaking the uncalcined shell powder in the leachate, drying the leachate after soaking for 40 ~ min for 40 min, the leachate is urea and sodium hydroxide aqueous solution, the concentration of the urea is 4 wt%, the concentration of the sodium hydroxide is 8 wt%, 2 ~ 4 parts, 2 ~ parts by mass of a vulcanizing agent, 0.3 ~.6 parts by mass of a vulcanizing aid, 18 parts of carbon black, ~ parts by mass of sulfur and 0.1 parts by mass of sulfur, and the requirement of the original composite compression set is reduced.
Description
Technical Field
The invention relates to ethylene propylene diene monomer, in particular to an ethylene propylene diene monomer sealing material with low compression set and a preparation method thereof.
Background
Ethylene propylene diene monomer is a copolymer of ethylene, propylene and a small amount of non-conjugated diene, represented by EPDM, and has excellent aging resistance such as ozone resistance, heat resistance, weather resistance and the like because the main chain thereof is composed of chemically stable saturated hydrocarbons and only contains unsaturated double bonds in the side chains, and can be widely used in the fields of automobile parts, waterproof materials for buildings, wire and cable sheaths, heat-resistant rubber tubes, adhesive tapes, automobile sealing parts and the like.
However, the main chain composed of the fully saturated hydrocarbon gives high compatibility, heat resistance and weather resistance to the ethylene propylene diene monomer, the bonding force between the inner molecular chains of the ethylene propylene diene monomer is small, relative sliding between the molecular chains is easy to occur, the bonding force inside the ethylene propylene diene monomer is low, and then the compression permanent deformation of the ethylene propylene diene monomer is large, and the ethylene propylene diene monomer has adverse influence on the field of sealing materials.
For example, when unmodified or non-specifically modified ethylene propylene diene monomer rubber is used on a sealing strip of an automobile window or door, the rubber is easily pressed by pressure kept or repeated for a long time, and the sealing strip is easily subjected to permanent deformation, so that the service life of the product is short and the product needs to be replaced frequently. Moreover, when the unmodified or non-specifically modified ethylene propylene diene monomer is used on sealing gaskets of pipelines and the like, under the action of long-term pressure, the rebound resilience is quickly reduced, the loss of the sealing effect is large, and the sealing leakage is easily caused.
Therefore, the ethylene propylene diene monomer needs to be correspondingly improved aiming at the compression permanent deformation, the high compatibility of the ethylene propylene diene monomer is adopted in the prior art, and a large amount of filler is mixed into the ethylene propylene diene monomer so as to reduce the compression permanent deformation of the ethylene propylene diene monomer. The method is mainly improved in a physical filling mode, the filling proportion of the method is large, and the proportion in the prior art reaches 40-55 wt%. But the influence range of the rubber on the mechanical property of the ethylene propylene diene monomer is large, the hardness of the ethylene propylene diene monomer is improved, the elastic modulus is increased, and the deformation property of the ethylene propylene diene monomer is greatly reduced, which is an unexpected result of the sealing material.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the ethylene propylene diene monomer sealing material with low compression set, which reduces the compression set of the ethylene propylene diene monomer sealing material while keeping the elasticity requirement of the original design.
The technical purpose of the invention is realized by the following technical scheme:
the ethylene propylene diene monomer sealing material with low compression set is characterized by comprising the following raw materials in parts by weight,
100 parts of ethylene propylene diene monomer, wherein 70-80 parts of the ethylene propylene diene monomer are maleic anhydride grafted ethylene propylene diene monomer;
15-30 parts of a filler, wherein the filler comprises freeze-thaw powder, the freeze-thaw powder accounts for more than 33 wt% of the filler, the particle size of the freeze-thaw powder is 400-600nm, and the preparation method of the freeze-thaw powder comprises the following steps: mixing uncalcined shell powder with leachate at the temperature of-15 to-14 ℃ in a mass ratio of 0.2 to 0.4:1, soaking the uncalcined shell powder in the leachate for 40 to 50min, and drying to obtain the catalyst, wherein the leachate is urea and sodium hydroxide aqueous solution, the concentration of the urea is 4 wt%, and the concentration of the sodium hydroxide is 8 wt%;
2-4 parts of a release agent;
2-4 parts of a vulcanizing agent;
0.3-0.6 part of a vulcanization assistant;
18-25 parts of carbon black;
800.1-0.4 parts of sulfur S.
By adopting the technical scheme, the freeze-thaw powder is obtained by soaking shell powder in an alkali/urea solution (leachate) at a low temperature, chitin in the shell powder is dissociated and dissolved out in the alkali/urea solution (leachate), a large number of microporous air passages are formed on the surface and inside of the shell powder after the chitin is dissociated and dissolved out, and meanwhile, small molecular polymeric chains of stably attached chitosan are formed on the surface of the shell powder and in the microporous air passages in the process of dissociating and dissolving out the chitin.
The small molecular polymer chain of the chitosan has cohesive property firstly, and can provide the internal cohesive property of the ethylene propylene diene monomer rubber from the physical aspect so as to reduce the compression permanent deformation of the ethylene propylene diene monomer rubber. Meanwhile, in the fused ethylene propylene diene monomer, part of amino groups (limited by conditions such as position resistance, reaction temperature and the like, but not all amino groups can react) on part of chitosan can react with maleic anhydride groups grafted in the ethylene propylene diene monomer grafted with maleic anhydride, so that polymeric carbon chains of the ethylene propylene diene monomer are combined with micromolecular polymeric chains of the chitosan, and then the adhesive connection between the ethylene propylene diene monomer and the freeze-thaw powder is enhanced, therefore, the freeze-thaw powder uniformly distributed in the ethylene propylene diene monomer sealing material is formed, the uniformly distributed reinforcing points are formed, the internal bonding force of the ethylene propylene diene monomer sealing material is enhanced, and the compression permanent deformation of the ethylene propylene diene monomer sealing material is reduced.
Furthermore, due to the fact that the freeze-thaw powder improves the benefit of the internal bonding force of the ethylene propylene diene monomer sealing material through physical and chemical double effects, the compression set of the ethylene propylene diene monomer sealing material is reduced, and the compression set of the ethylene propylene diene monomer sealing material is reduced in a mode of improving the elastic modulus and the compressive capacity of the ethylene propylene diene monomer sealing material and reducing the overall deformation, instead of the mode of reducing the compression set of the ethylene propylene diene monomer sealing material through a large amount of fillers in the prior art, the requirement on the addition amount of the fillers is low, and the performance variation quantity of the ethylene propylene diene monomer sealing material such as the.
Meanwhile, the ethylene propylene diene monomer is not completely maleic anhydride grafted ethylene propylene diene monomer, but part of the ethylene propylene diene monomer is raw rubber or oil-filled rubber, the internal cohesive property reinforcing effect of reinforcing points formed by freeze-thaw powder in the ethylene propylene diene monomer sealing material is adjusted, so that the compression permanent deformation of the ethylene propylene diene monomer sealing material is reduced, and the ethylene propylene diene monomer sealing material keeps the elastic requirement of the original design. The use requirements of the ethylene propylene diene monomer rubber sealing material in corresponding fields such as automobile window sealing strips and pipeline sealing rings are met, and the ethylene propylene diene monomer rubber sealing material has good elastic sealing performance and good flexibility and deformability.
The invention is further configured to: the filler also comprises calcined powder, the proportion of the calcined powder in the filler is less than 45.5wt%, the particle size of the calcined powder is 700-800nm, and the preparation method of the calcined powder comprises the following steps: calcining the uncalcined shell powder at high temperature, and then mixing the uncalcined shell powder with the raw materials in a mass ratio of 1: 1, mixing calcined shell powder and a urea solution, soaking for 5-8 min, filtering, heating and drying to obtain the urea-containing urea solution, wherein the concentration of urea in the urea solution is 2-3 wt%.
By adopting the technical scheme, the benefit of the internal binding force of the ethylene propylene diene monomer sealing material is improved by the physical and chemical double effects of freeze-thaw powder, and meanwhile, the freeze-thaw powder is used as a filler singly obtained by experimental tests, and the reduction of the compression permanent deformation of the obtained ethylene propylene diene monomer sealing material is limited because the addition amount of the freeze-thaw powder is increased. The properties such as elastic modulus, compressive capacity, hardness and the like of the EPDM rubber sealing material can be still increased along with the increase of the dosage of the freeze-thaw powder, wherein after the dosage of the freeze-thaw powder reaches a certain amount (the total content in the raw materials is more than 44 wt%), the compression permanent deformation of the EPDM rubber is not reduced, and the EPDM rubber is hardened along with the increase of the dosage of the freeze-thaw powder.
The calcined powder is used together with freeze-thaw powder, so that the compression permanent deformation of the ethylene propylene diene monomer sealing material can be further reduced on the premise of less addition amount, and the good elastic sealing performance and good flexibility and deformability of the ethylene propylene diene monomer sealing material are ensured.
The invention is further configured to: the filler also comprises white carbon black, wherein the proportion of the white carbon black in the filler is less than 40 wt%, and the particle size of the white carbon black is 700-800 nm; the ethylene propylene diene monomer sealing material further comprises 2-4 parts of polysiloxane.
By adopting the technical scheme, the maximum white carbon black in mass part is 12 parts, the hardness and the compression resistance of the ethylene propylene diene monomer are adjusted, and the compatibility of the white carbon black and the ethylene propylene diene monomer is enhanced by adding polysiloxane.
The invention is further configured to: the silane coupling agent is hydroxyl-terminated polysiloxane.
By adopting the technical scheme, the hydroxyl of the hydroxyl-terminated polysiloxane can be subjected to a grafting reaction with maleic anhydride for ring opening, and competes with amino on chitosan for grafting with maleic anhydride, so that the length between the molecular chain joints of chitosan on an ethylene propylene diene monomer polymerization chain is increased, the improvement of the self-adhesiveness to the hardness and the elastic modulus of the ethylene propylene diene monomer is slowed down, and the good deformability of the ethylene propylene diene monomer sealing material is ensured.
The invention is further configured to: the raw materials of the medicine comprise the following components in parts by mass,
100 parts of ethylene propylene diene monomer, wherein 70 parts of the ethylene propylene diene monomer are maleic anhydride grafted ethylene propylene diene monomer;
28 parts of filler, wherein the filler comprises freeze-thaw powder, calcined powder and white carbon black;
the particle size of the freeze-thaw powder is 400-600nm, and the preparation method of the freeze-thaw powder comprises the following steps: mixing uncalcined shell powder with leachate at the temperature of-15 to-14 ℃ in a mass ratio of 0.2 to 0.4:1, soaking the uncalcined shell powder in the leachate for 40 to 50min, and drying to obtain the catalyst, wherein the leachate is urea and sodium hydroxide aqueous solution, the concentration of the urea is 4 wt%, and the concentration of the sodium hydroxide is 8 wt%; the particle size of the calcined powder is 700-800nm, and the preparation method of the calcined powder comprises the following steps: calcining the uncalcined shell powder at high temperature, and then mixing the uncalcined shell powder with the raw materials in a mass ratio of 1: 1, mixing calcined shell powder and a urea solution, soaking for 5-8 min, filtering, heating and drying to obtain the urea, wherein the concentration of urea in the urea solution is 2-3 wt%;
the particle size of the white carbon black is 700-800 nm;
the mass ratio of the freeze-thaw powder to the calcined powder to the white carbon black is 10:8: 10;
3 parts of a release agent;
2 parts of a vulcanizing agent;
and 0.5 part of a vulcanization aid.
By adopting the technical scheme, the ethylene propylene diene monomer sealing material prepared from the raw materials according to the proportion has good flexibility and deformability, is low in compression permanent deformation, and meets the use requirements of the ethylene propylene diene monomer sealing material in corresponding fields such as automobile window sealing strips and pipeline sealing rings.
The invention is further configured to: the ethylene propylene diene monomer rubber is oil-filled ethylene propylene diene monomer rubber except the maleic anhydride grafted ethylene propylene diene monomer rubber.
By adopting the technical scheme, the ethylene propylene diene monomer rubber part is the oil-filled ethylene propylene diene monomer rubber, so that the flexibility of the obtained ethylene propylene diene monomer rubber sealing material is improved, the compression permanent deformation is reduced, and the possibility of surface pressure loss of the ethylene propylene diene monomer rubber sealing material is reduced.
The invention is further configured to: the vulcanizing agent is zinc oxide, and the zinc oxide is prepared from zinc oxide powder and zinc oxide tetrapod-like crystal whisker according to the mass ratio of 1: 0.8.
By adopting the technical scheme, the zinc oxide powder and the zinc oxide tetrapod-like crystal whisker have different vulcanization catalysis trends respectively, and the compression permanent deformation of the obtained ethylene propylene diene monomer sealing material can be further reduced according to the composite vulcanizing agent.
Aiming at the defects in the prior art, the invention aims to provide a preparation method of an ethylene propylene diene monomer sealing material with low compression permanent deformation, and the ethylene propylene diene monomer sealing material with good elastic sealing performance and good flexibility and deformability is produced and prepared.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of an ethylene propylene diene monomer sealing material with low compression set comprises the following steps,
s1: weighing 100 parts of ethylene propylene diene monomer according to the mass parts, adding the ethylene propylene diene monomer into an internal mixer, stirring and heating for 50-60 s, and heating to 60 ℃;
s2: after the temperature in an internal mixer reaches 60 ℃, weighing and adding 15-30 parts of filler, 2-4 parts of release agent, 2-4 parts of vulcanizing agent, 0.3-0.6 part of vulcanization assistant and 18-25 parts of carbon black according to parts by weight, continuing to heat and stir for 100-120S, heating to 90 ℃, then heating to 800.1-0.4 part of sulfur, continuing to stir, stopping stirring and heating when the temperature of the internal mixer reaches 120 ℃, and discharging rubber to obtain mixed rubber;
s3: thinly passing the rubber compound on an open mill for 2-3 times, and discharging rubber strips;
s4: and cooling the rubber strip to 20-35 ℃ by air cooling equipment to obtain the ethylene propylene diene monomer.
By adopting the technical scheme, the ethylene propylene diene monomer sealing material with low compression set is produced and provided, the compression set of the ethylene propylene diene monomer sealing material is reduced, the ethylene propylene diene monomer sealing material keeps the elastic requirement of the original design, the use requirements of the ethylene propylene diene monomer sealing material in the corresponding fields such as automobile window sealing strips and pipeline sealing rings are met, and the ethylene propylene diene monomer sealing material has good elastic sealing performance and good flexibility and deformability.
In conclusion, the invention has the following beneficial effects:
the ethylene propylene diene monomer sealing material with low compression set is prepared, the compression set of the ethylene propylene diene monomer sealing material is reduced, meanwhile, the ethylene propylene diene monomer sealing material meets the elastic requirement of the original design, so that the use requirement of the ethylene propylene diene monomer sealing material in the corresponding fields such as automobile window sealing strips and pipeline sealing rings is met, and the ethylene propylene diene monomer sealing material has good elastic sealing performance and good flexibility and deformability.
Detailed Description
In the examples 1 to 6, the following examples were conducted,
the ethylene propylene diene monomer sealing material with low compression set consists of the following components in weight portion,
100 parts of ethylene-propylene-diene monomer rubber,
15-30 parts of a filler,
2-4 parts of a release agent,
2-4 parts of a vulcanizing agent,
0.3 to 0.6 part of a vulcanization assistant,
18-25 parts of carbon black,
800.1 to 0.4 portion of sulfur S,
2-4 parts of a silane coupling agent.
70-80 parts of ethylene propylene diene monomer is maleic anhydride grafted ethylene propylene diene monomer, and the balance is oil-extended ethylene propylene diene monomer.
The filler comprises one or more of freeze-thaw powder, calcined powder and white carbon black, wherein the proportion of the freeze-thaw powder in the filler is more than 33 wt%, the proportion of the calcined powder in the filler is less than 45.5wt%, and the proportion of the white carbon black in the filler is less than 40 wt%.
The particle size of the freeze-thaw powder is 400-600nm, and the preparation method of the freeze-thaw powder comprises the following steps: mixing the uncalcined shell powder with a leachate at the temperature of-15 to-14 ℃ in a mass ratio of 0.2 to 0.4:1, soaking the uncalcined shell powder in the leachate for 40 to 50min, and drying to obtain the catalyst. Wherein the leaching solution is urea and sodium hydroxide aqueous solution, the concentration of the urea is 4 wt%, and the concentration of the sodium hydroxide is 8 wt%.
The particle size of the calcined powder is 700-800nm, and the preparation method of the calcined powder comprises the following steps: calcining the uncalcined shell powder at high temperature, and then mixing the uncalcined shell powder with the raw materials in a mass ratio of 1: 1, mixing calcined shell powder and a urea solution, soaking for 5-8 min, filtering, and heating and drying to obtain the urea-containing aqueous solution, wherein the concentration of urea in the urea solution is 2-3 wt%.
The release agent is release agent L-24.
The vulcanizing agent is zinc oxide, and the zinc oxide is one or more of zinc oxide powder and zinc oxide tetrapod-like whiskers.
The vulcanization assistant is ethylene glycol methacrylate.
The sulfur is sulfur S-80.
The silane coupling agent is hydroxyl-terminated polysiloxane.
The preparation method of the ethylene propylene diene monomer sealing material with low compression set comprises the following steps,
s1: weighing 100 parts of ethylene propylene diene monomer according to the mass parts, adding the ethylene propylene diene monomer into an internal mixer, stirring and heating for 50-60 s, and heating to 60 ℃;
s2: after the temperature in an internal mixer reaches 60 ℃, weighing and adding 15-30 parts of filler, 2-4 parts of release agent, 2-4 parts of vulcanizing agent, 0.3-0.6 part of vulcanization assistant, 18-25 parts of carbon black and other raw materials according to parts by weight, continuing to heat and stir for 100-120S, heating to 90 ℃, then heating sulfur S-800.1-0.4 part, continuing to stir, stopping stirring and heating when the temperature of the internal mixer reaches 120 ℃, and discharging rubber to obtain a rubber compound;
s3: thinly passing the rubber compound on an open mill for 2-3 times, and discharging rubber strips;
s4: and cooling the rubber strip to 20-35 ℃ by air cooling equipment to obtain the ethylene propylene diene monomer.
The preparation of the ethylene propylene diene monomer sealing material was carried out according to the above preparation method to obtain examples 1 to 6. Specific parameters of examples 1 to 6 are shown in Table I.
Comparative examples 1 to 5 were also provided.
In the comparative example 1,
an ethylene-propylene-diene monomer rubber sealing material is based on example 4, and is characterized in that the amount of the filler is zero.
In a comparative example 2,
an ethylene propylene diene monomer sealing material is based on the embodiment 4, and is characterized in that the amount of freeze-thaw powder is zero.
In a comparative example 3,
an ethylene propylene diene monomer rubber sealing material is characterized in that the calcined powder amount is zero based on example 4.
In a comparative example 4,
an ethylene-propylene-diene monomer rubber sealing material is based on example 4, and is distinguished in that the filler is calcined powder only and is used in an amount of 28 parts.
In a comparative example 5,
an ethylene propylene diene monomer sealing material is based on example 4, and is characterized in that the filler comprises 18 parts of calcined powder and 12 parts of white carbon black.
In a comparative example 6,
based on example 4, the ethylene propylene diene monomer sealing material is characterized in that the amount of the filler is 28 parts of freeze-thaw powder.
The hardness, elastic modulus, tensile strength, tensile fracture rate and compression set of the ethylene propylene diene monomer sealing materials obtained in examples 1 to 6 and comparative examples 1 to 5 were measured, and the results are shown in Table II.
Wherein the hardness is as defined in part 1 of GB/T531.1 Press hardness test method for vulcanizates or thermoplastics: the shore durometer method was used for testing.
The elastic modulus is obtained by testing the quantitative tensile quantity of 100% at normal temperature.
The tensile strength and the tensile fracture rate are tested according to the testing method recorded in GB/T528 vulcanized rubber or thermoplastic rubber tensile stress strain performance, and the sample adopts type I.
The compression set is measured by a test method in GB/T7759 vulcanized rubber or thermoplastic rubber compression set measurement under normal temperature, high temperature and low temperature, the measurement conditions are that the temperature is 70 ℃, the temperature is 24 hours, and the compression ratio is 25 percent.
Watch two
| hardness/HA | Modulus of elasticity/MPa | Tensile strength | Elongation at break | Compression set/%) | |
| Example 1 | 60 | 1.6 | 8.7 | 386 | 19.4 |
| Example 2 | 62 | 1.65 | 8.9 | 389 | 16.2 |
| Example 3 | 61 | 1.8 | 8.8 | 386 | 19.1 |
| Example 4 | 60 | 1.65 | 8.8 | 388 | 12.6 |
| Example 5 | 63 | 1.85 | 8.9 | 385 | 18.5 |
| Example 6 | 61 | 1.65 | 8.7 | 393 | 17.5 |
| Comparative example 1 | 56 | 1.5 | 8.5 | 365 | 32.7 |
| Comparative example 2 | 70 | 2.15 | 8.6 | 370 | 28.3 |
| Comparative example 3 | 68 | 2.25 | 8.7 | 372 | 19.6 |
| Comparative example 4 | 76 | 2.45 | 8.6 | 374 | 25.2 |
| Comparative example 5 | 78 | 2.35 | 8.5 | 371 | 26.7 |
| Comparative example 6 | 68 | 1.98 | 8.7 | 376 | 22.4 |
As can be seen from the above table, in comparison with the comparative examples 1 to 6 and the comparative examples 1 and 2, the freeze-thaw powder has double physical and chemical effects to improve the benefit of the internal bonding force of the epdm rubber sealing material and reduce the compression set of the epdm rubber sealing material, rather than the prior art that the elastic modulus and the compressive strength of the epdm rubber sealing material are improved by a large amount of filler, and the compression set of the epdm rubber sealing material is reduced by reducing the overall deformation, so that the requirement on the addition amount of the filler is low, and the variation of the properties such as the elastic modulus, the compressive strength and the hardness of the epdm rubber sealing material is small.
Comparing the example 4 with the comparative example 3, the comparative example 5 and the comparative example 7, wherein all the ethylene propylene diene monomer is not maleic anhydride grafted ethylene propylene diene monomer, part of the ethylene propylene diene monomer is raw rubber or oil-extended rubber, the internal cohesive property reinforcing effect of reinforcing points formed by freeze-thaw powder in the ethylene propylene diene monomer sealing material is adjusted, so that the compression permanent deformation of the ethylene propylene diene monomer sealing material is reduced, and the ethylene propylene diene monomer sealing material meets the elastic requirement of the original design. The use requirements of the ethylene propylene diene monomer rubber sealing material in corresponding fields such as automobile window sealing strips and pipeline sealing rings are met, and the ethylene propylene diene monomer rubber sealing material has good elastic sealing performance and good flexibility and deformability.
In addition, in the comparative example 4, the example 2 and the comparative example 6, the hardness and the compression resistance of the ethylene propylene diene monomer rubber can be adjusted by adding the white carbon black in parts by mass.
In the case of the example 7, the following examples are given,
an EPDM sealing material with low compression set is based on example 4 and is distinguished by the fact that the catalyst used is zinc sulfide powder.
In the case of the example 8, the following examples are given,
an ethylene-propylene-diene monomer rubber sealing material with low compression set is based on example 4 and is characterized in that zinc sulfide whiskers are used as a catalyst.
In the case of the example 9, the following examples are given,
based on example 4, the ethylene propylene diene monomer sealing material with low compression set is characterized in that 70-80 parts of the ethylene propylene diene monomer is maleic anhydride grafted ethylene propylene diene monomer, and the balance is rubber ethylene propylene diene monomer.
In the light of the above example 10,
an ethylene-propylene-diene rubber sealing material having a low compression set is distinguished, based on example 4, in that the silicon coupling agent is a methyl-terminated polysiloxane.
In the case of the embodiment 11, the following examples are given,
an ethylene-propylene-diene monomer rubber sealing material having a low compression set was obtained in the same manner as in example 4 except that the amount of the silicon coupling agent was 0.
The hardness, elastic modulus, tensile fracture rate and compression set of the ethylene propylene diene monomer sealing materials obtained in examples 7 to 12 were measured, and the results are shown in table three.
As is clear from the second and third tables, in comparative examples 4, 7 and 8, the zinc oxide powder and the zinc oxide tetrapod-like whiskers each had a different tendency to undergo vulcanization catalysis, and the compression set of the resulting ethylene-propylene-diene rubber sealing material was further reduced by the above-mentioned composite vulcanizing agent.
Comparing examples 4 and 9, it is known that the ethylene propylene diene monomer rubber part is oil-filled ethylene propylene diene monomer rubber, so that the flexibility of the obtained ethylene propylene diene monomer rubber sealing material is improved, the compression permanent deformation is reduced, and the possibility of surface pressure loss of the ethylene propylene diene monomer rubber sealing material is reduced.
It can be known from comparative examples 4, 10 and 11 that the hydroxyl group of the hydroxyl-terminated polysiloxane can be subjected to ring opening reaction with maleic anhydride grafting reaction, and competes with the amino group on the chitosan for maleic anhydride grafting, so that the length between the molecular chain joints of the chitosan on the polymer chain of the ethylene propylene diene monomer is increased, the increase of the self-adhesiveness to the hardness and the elastic modulus of the ethylene propylene diene monomer is slowed down, and the good deformability of the ethylene propylene diene monomer sealing material is ensured.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (8)
1. The ethylene propylene diene monomer sealing material with low compression set is characterized by comprising the following raw materials in parts by weight,
100 parts of ethylene propylene diene monomer, wherein 70-80 parts of the ethylene propylene diene monomer are maleic anhydride grafted ethylene propylene diene monomer;
15 ~ 30 parts of filler, wherein the filler comprises freeze-thaw powder, the freeze-thaw powder accounts for more than 33 wt% in the filler, the particle size of the freeze-thaw powder is 400-600nm, and the preparation method of the freeze-thaw powder comprises the steps of mixing uncalcined shell powder with leachate at-15 ~ -14 ℃ according to the mass ratio of 0.2 ~ 0.4:1, soaking the uncalcined shell powder in the leachate for 40 ~ 50min, and drying to obtain the leachate, wherein the leachate is urea and sodium hydroxide aqueous solution, the concentration of the urea is 4 wt%, and the concentration of the sodium hydroxide is 8 wt%;
2 ~ 4 parts of a release agent;
2 ~ 4 parts of a vulcanizing agent;
0.3 part of vulcanization assistant 0.3 ~ 0.6.6 parts;
18 parts of carbon black 18 ~ 25;
0.4 part of sulfur S-800.1 ~ 0.4.
2. The ethylene propylene diene monomer sealing material with low compression set as claimed in claim 1, wherein the filler further comprises calcined powder, the calcined powder accounts for less than 45.5wt% of the filler, the particle size of the calcined powder is 700-800nm, the calcined powder is prepared by mixing calcined shell powder and urea solution according to the mass ratio of 1: 1 after calcining the uncalcined shell powder at high temperature, soaking for 5 ~ 8min, filtering, heating and drying, and the urea concentration in the urea solution is 2 ~ 3 wt%.
3. The ethylene propylene diene monomer sealing material with low compression set as claimed in claim 1, wherein the filler further comprises silica, the silica accounts for less than 40 wt% of the filler, the silica has a particle size of 700-800nm, and the ethylene propylene diene monomer sealing material further comprises 2 ~ 4 parts of a silane coupling agent.
4. The sealant material of claim 3 wherein said silane coupling agent is an epoxy group-containing siloxane.
5. The EPDM sealing material with low compression set of claim 1 wherein the raw materials include the following components and their mass portions,
100 parts of ethylene propylene diene monomer, wherein 70 parts of the ethylene propylene diene monomer are maleic anhydride grafted ethylene propylene diene monomer;
28 parts of filler, wherein the filler comprises freeze-thaw powder, calcined powder and white carbon black;
the particle size of the freeze-thaw powder is 400-600nm, and the preparation method of the freeze-thaw powder comprises the steps of mixing uncalcined shell powder with leachate at the temperature of-15 ~ -14 ℃ in a mass ratio of 0.2 ~ 0.4.4: 1, soaking the uncalcined shell powder in the leachate for 40 ~ 50min, and drying the soaked uncalcined shell powder to obtain the freeze-thaw powder, wherein the leachate is urea and an aqueous solution of sodium hydroxide, the concentration of the urea is 4 wt%, and the concentration of the sodium hydroxide is 8 wt%;
the particle size of the calcined powder is 700-800nm, and the calcined powder is prepared by calcining uncalcined shell powder at high temperature, mixing the calcined shell powder and a urea solution according to the mass ratio of 1: 1, soaking for 5 ~ 8min, filtering, heating and drying, wherein the urea concentration in the urea solution is 2 ~ 3 wt%;
the particle size of the white carbon black is 700-800 nm;
the mass ratio of the freeze-thaw powder to the calcined powder to the white carbon black is 10:8: 10;
3 parts of a release agent;
2 parts of a vulcanizing agent;
and 0.5 part of a vulcanization aid.
6. The EPDM sealing material with low compression set of claim 1 wherein the balance of the EPDM, excluding the maleic anhydride grafted EPDM, is oil-extended EPDM.
7. The ethylene propylene diene monomer rubber sealing material with low compression set of claim 1, wherein the vulcanizing agent is zinc oxide, and the zinc oxide is prepared from zinc oxide powder and zinc oxide tetrapod-like whiskers according to a mass ratio of 1: 0.8.
8. The method for producing an EPDM sealing material with low compression set as claimed in claim 1 ~ 7, wherein the method comprises the steps of,
s1, weighing 100 parts of ethylene propylene diene monomer according to the parts by weight, adding the ethylene propylene diene monomer into an internal mixer, stirring and heating for 50 ~ 60S, and heating to 60 ℃;
s2, after the temperature in the internal mixer reaches 60 ℃, weighing and adding 15 ~ 30 parts of filler, 2 ~ 4 parts of release agent, 2 ~ 4 parts of vulcanizing agent, 0.3 ~ 0.6.6 parts of vulcanization assistant and 18 ~ 25 parts of carbon black according to the parts by weight, continuously heating and stirring for 100 ~ 120S, heating to 90 ℃, then heating sulfur S-800.1 ~ 0.4 parts, continuously stirring, stopping stirring and heating when the temperature of the internal mixer reaches 120 ℃, and discharging rubber to obtain rubber compound;
s3, thinly passing the mixed rubber on an open mill for 2 ~ 3 times, and discharging rubber strips;
and S4, cooling the rubber strip to 20 ~ 35 ℃ by air cooling equipment to obtain the ethylene propylene diene monomer.
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Application publication date: 20191231 |