CN115651324A - Wide-temperature-range high-damping composite rubber material and preparation method thereof - Google Patents
Wide-temperature-range high-damping composite rubber material and preparation method thereof Download PDFInfo
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- CN115651324A CN115651324A CN202211338346.3A CN202211338346A CN115651324A CN 115651324 A CN115651324 A CN 115651324A CN 202211338346 A CN202211338346 A CN 202211338346A CN 115651324 A CN115651324 A CN 115651324A
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Abstract
The invention relates to the technical field of damping materials, in particular to a wide-temperature-range high-damping composite rubber material and a preparation method thereof. The composite rubber material comprises: raw rubber and a damping agent with the weight ratio of 2.5-5; the raw rubber consists of butyl rubber, polynorbornene rubber and ethylene propylene diene monomer rubber; the weight percentage of the ethylene propylene diene monomer in the raw rubber is 8-20%; the damping agent is at least one of terpene resin or modified terpene resin. The composite rubber material has good mechanical property, bonding property and excellent damping property, and simultaneously has a wider temperature range. Moreover, the preparation method of the composite rubber material is simple, and the composite rubber material is easy to popularize and use as a rubber elastic element material in the fields of buildings, bridges and the like.
Description
Technical Field
The invention relates to the technical field of damping materials, in particular to a wide-temperature-range high-damping composite rubber material and a preparation method thereof.
Background
With the continuous development of the seismic isolation technology, the laminated rubber support is widely applied in structural engineering, and mainly comprises a natural rubber support, a lead core rubber support, a high-damping rubber support and the like. The damping ratio of the natural rubber support is lower, only 0.02-0.04, the damping performance is poorer, and a viscoelastic damper and the like are required to be matched when the natural rubber support is used. The damping ratio of the lead core rubber support can reach 0.12-0.15, but in the production process, heavy metal pollution is easily generated, the current civil engineering construction guidance concept of environment-friendly and green development is not met, and in the use process, the lead core in the support is easily subjected to deformation damage caused by shear fatigue (experiments show that after 5000 times of small deformation, the damping performance of the lead core is reduced by 25%). Different from the former two, the high-damping rubber support has better damping performance, the damping ratio is about 0.12-0.20, no pollution and low energy consumption are realized, but the effective unification of high damping and low modulus is difficult to realize.
Under normal conditions, the damping performance of the halogenated butyl material is superior to that of other materials, but the damping factor is small at normal temperature, the effective damping temperature range of tan delta larger than or equal to 0.4 is only between-52 ℃ and 15 ℃, the damping ratio is low, the bonding performance is poor, and the use requirement of the high-damping rubber support cannot be effectively met. The traditional carbon black filler has environmental hazards of high energy consumption, high pollution and the like, so that the traditional halogenated butyl material is greatly controversial and objected to as a raw material of a high-damping rubber support in the using process.
Therefore, how to overcome the above disadvantages and defects and provide a wide temperature range and high damping composite rubber material becomes a technical problem to be solved urgently in the field.
Disclosure of Invention
First, the present invention provides a composite rubber material comprising: raw rubber and a damping agent in a weight ratio of 2.5-5;
the raw rubber consists of butyl rubber, polynorbornene rubber and ethylene propylene diene monomer rubber;
the weight percentage of the ethylene propylene diene monomer in the raw rubber is 8-20%;
the damping agent is at least one of terpene resin or modified terpene resin.
According to the invention, under the composite rubber material system, the raw rubber composed of the butyl rubber, the polynorbornene rubber and the ethylene propylene diene monomer rubber can enable the damping peak value (loss factor peak value) to move to the right, effectively improve the damping performance of the rubber material at normal temperature and high temperature, and further widen the effective damping temperature range of the rubber material.
Moreover, the glass transition temperatures of the raw rubber and the damping agent have larger difference, and when the raw rubber and the damping agent are mixed according to the proportion, the overall damping factor of the composite rubber material can be obviously improved, and the effective damping temperature range of the low-temperature section and the high-temperature section of the rubber material is effectively widened. Meanwhile, under the condition of raw rubber and the damping agent in the proportion, the wettability of the rubber material and the metal material can be obviously improved, so that the damping agent can simultaneously form a hydrogen bond effect with the rubber and the adhesive (the adhesive is generally coated on the surface of the metal when the rubber is bonded with the metal), the bonding property of the rubber material and the metal can be further improved on the premise of ensuring the high damping property of the rubber material, and the bonding strength of the rubber material and the metal can be improved by over 60 percent.
The composite rubber material has good mechanical property, excellent damping property and wider effective damping temperature range.
In a preferred embodiment of the present invention, the butyl rubber is 65 to 75% by weight of the raw rubber.
In a preferred embodiment of the present invention, the weight ratio of the butyl rubber, the polynorbornene rubber and the ethylene propylene diene monomer rubber is 3-9: 0.4-4.
The raw rubber formed in the proportion can be better cooperated with a damping agent, the mechanical property and the damping property of the composite rubber material are further improved, and the damping temperature range is remarkably widened. Tests prove that the composite rubber material has the first loss factor peak value of more than 1.5 at the temperature of 0 ℃, the second loss factor peak value of more than 0.9 at the temperature of 50 ℃ and the effective damping temperature range of tan delta more than or equal to 0.4 widened to-70 ℃.
In a preferred embodiment of the present invention, the softening point of the damping agent is 80 ℃ to 120 ℃.
As a preferred embodiment of the present invention, the modified terpene resin is at least one of a phenol-formaldehyde modified terpene resin, a phenol-modified terpene resin, and an aromatic hydrocarbon modified terpene resin.
As a preferred embodiment of the present invention, the butyl rubber is chlorinated butyl rubber and/or brominated butyl rubber.
As a preferred embodiment of the present invention, the composite rubber material further comprises: a reinforcing filler;
the reinforcing filler is at least one of graphene, graphene oxide, graphite powder, single-arm or multi-arm carbon nano tubes, AO-2246, fumed silica, flaky mica powder, kaolin, argil and montmorillonite;
the weight ratio of the reinforcing filler to the raw rubber is 1;
preferably, the weight ratio of the reinforcing filler to the butyl rubber, the polynorbornene rubber and the ethylene propylene diene monomer is 2-5: 3 to 9:0.4 to 4:1.
the invention further discovers that the maximum damping factor of the composite rubber material can be greatly improved by adopting the reinforcing filler with a proper proportion in the system of the raw rubber and the damping agent, and the defects of high pollution, high energy consumption and the like of the traditional carbon black material can be effectively reduced.
Preferably, the reinforcing filler is single-arm carbon nanotubes or graphene.
If reinforcing fillers such as kaolin and mica powder are used to cause insufficient reinforcing effect, carbon black should be used in combination, and the best effect is obtained with the N330 grade carbon black.
The vulcanizing agent and the accelerator in the present invention are not particularly limited, and the type and amount used in the production of a usual halogenated butyl rubber can be used, and when the rubber compound is required to have high-temperature resistance, a resin vulcanization system (for example, t-butylphenol formaldehyde resin (2402 resin), reactive phenol resin, p-t-octylphenol formaldehyde resin, etc.) is preferable. The present invention can use accelerators commonly used for rubbers such as BZ, CZ and TMTD.
In the concrete implementation, various additives such as processing aids, scorch retarders, etc. may be added to the composite rubber material of the present invention, if necessary.
As a preferred embodiment of the invention, the composite rubber material comprises the following components in parts by weight:
100 portions of crude rubber, 20 to 40 portions of damping agent, 3 to 10 portions of zinc oxide, 1 to 3 portions of stearic acid, 0.5 to 2 portions of magnesium oxide, 40 to 80 portions of reinforcing filler, 1 to 5 portions of vulcanizing agent and 4 to 10 portions of accelerant.
As a preferred embodiment of the invention, the composite rubber material comprises the following components in parts by weight:
65-75 parts of butyl rubber, 8-20 parts of polynorbornene rubber, 8-20 parts of ethylene propylene diene monomer, 20-40 parts of damping agent, 3-10 parts of zinc oxide, 1-3 parts of stearic acid, 0.5-2 parts of magnesium oxide, 40-50 parts of reinforcing filler, 1-5 parts of vulcanizing agent and 4-10 parts of accelerator.
Preferably, the accelerator is at least one of BZ, CZ, TMTD and DTDM.
Preferably, the accelerator is a system with a medium-speed accelerator and an overspeed accelerator as main accelerators.
Further, the present invention provides a method for preparing the composite rubber material in any one of the above embodiments, comprising:
(1) Plasticating the raw rubber for 3-5min at 50-80 ℃;
(2) Mixing the plasticated raw rubber with other components, and then carrying out banburying at a temperature higher than the softening point of the damping agent;
(3) Performing thin-passing, triangular-wrapping and discharging on the rubber composite material subjected to banburying;
(4) And vulcanizing the discharged rubber composite material at the temperature of 140-170 ℃ to obtain the rubber composite material.
As a preferred embodiment of the present invention, the plastication is carried out for 1 to 3min.
In a preferred embodiment of the invention, the temperature for the internal mixing is from 100 ℃ to 130 ℃.
As a preferred embodiment of the invention, triangular bags can be formed and discharged after the thin passing is carried out for 1 to 2 times.
In the specific implementation process, the vulcanization temperature is kept between 140 ℃ and 170 ℃ according to the experimental result of the rotor-free vulcameter test, and the time is controlled to be 20-45 minutes.
As a more preferred embodiment of the present invention, a method for producing a composite rubber material comprises:
(1) Plasticating the raw rubber for 3-5min at 50-80 ℃; then, internally mixing the plasticated raw rubber and a damping agent at a temperature higher than the softening point of the damping agent so that the damping agent is completely softened and uniformly dispersed in a rubber matrix material;
(2) Adding zinc oxide, stearic acid and magnesium oxide for banburying, so that the three small materials are uniformly dispersed in the rubber matrix material;
(3) Adding a reinforcing filler for banburying, so that the reinforcing filler is uniformly dispersed in the rubber matrix material;
(4) After the rubber material is cooled to about 70 ℃, adding a vulcanizing agent, a peroxide crosslinking agent and an accelerator for banburying, so that various auxiliaries are uniformly dispersed in the rubber matrix material;
(5) Vulcanizing the discharged rubber composite material at 140-170 ℃ to obtain the rubber composite material;
in the specific implementation process, the mixing is carried out until the complete feeding is achieved.
And (4) observing that the rubber material completely eats powder after discharging in the step (3), and if reinforcing agent is left in the internal mixer or reinforcing agent is left on the surface of the rubber material in a block or sheet shape, returning the rubber material to the internal mixer for continuous internal mixing.
In the specific implementation process, in order to prevent rubber materials from being scrapped due to the fact that the rubber vulcanizing agent is vulcanized in advance in the banburying process, the temperature of the banbury mixer needs to be adjusted to 70 +/-5 ℃.
In the specific implementation process, the rubber discharged in the step (4) is placed for more than 24 hours and then is vulcanized.
Preferably, the discharged rubber composite is pressed into a sheet of about 2mm by an open mill and vulcanized on a flat vulcanizing machine.
Preferably, the step (1) is banburied for 2-5 min at the temperature of 100-120 ℃; or, banburying in the step (2) for 1-3 min; or, banburying in the step (3) for 3-10 min; or, banburying in the step (4) for 1-3 min.
Compared with the prior art, the invention has the beneficial effects that:
the composite rubber material has good mechanical property, bonding property and excellent damping property, and simultaneously has a wider temperature range. Moreover, the preparation method of the composite rubber material is simple, and the composite rubber material is easy to popularize and use as a rubber elastic element material in the fields of buildings, bridges and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless otherwise defined, 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 herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The embodiment provides a composite rubber material, which specifically comprises the following components:
66.67g of brominated butyl rubber, 16.67g of polynorbornene rubber, 16.67g of ethylene propylene diene monomer, 10g of zinc oxide, 3g of stearic acid, 2g of magnesium oxide, 2g of sulfur, 2g of BZ, 3g of CZ, 3g of DCP, 1g of TMTD, 3g of DMDT, 2402 30g of phenolic resin, 5g of single-walled carbon nanotube, 10g of graphite powder, AO-2246, 10g of N330, and 15g of the single-walled carbon nanotube.
The preparation process comprises the following steps:
(1) Firstly, respectively putting brominated butyl rubber, polynorbornene rubber and ethylene propylene diene monomer rubber into an open mill, plastifying for 3min at 70 ℃, then adding the plastified rubber and damping agent phenolic resin into an internal mixer, and mixing for 2min at the mixing temperature of 100 ℃, so that the phenolic resin is completely softened and uniformly dispersed in a rubber matrix.
(2) Then adding premixed zinc oxide, stearic acid and magnesium oxide for banburying for 2min.
(3) And then adding a reinforcing filler for banburying for 8min to uniformly disperse the reinforcing filler in the rubber matrix material, and stopping cooling after the rubber is observed to be completely eaten.
(4) Cooling to about 70 ℃, adding a vulcanizing agent, a peroxide crosslinking agent and an accelerant which are mixed uniformly in advance, and banburying for 2min to uniformly disperse various auxiliaries in the rubber matrix material.
(5) And (4) sheet discharging is carried out on an open mill with the roller spacing kept at 2mm, and cooling is carried out to obtain the master batch.
(6) And (3) standing the master batch for 24 hours, and then putting the master batch into a vulcanizing machine to vulcanize for 30min at 150 ℃ to obtain the composite rubber material.
Example 2
The embodiment provides a composite rubber material, which specifically comprises the following components:
16.67g of brominated butyl rubber, 66.67g of polynorbornene rubber, 16.67g of ethylene propylene diene monomer, 10g of zinc oxide, 3g of stearic acid, 2g of magnesium oxide, 2g of sulfur, 2g of BZ, 3g of CZ, 3g of DCP, 1g of TMTD, 3g of DMDT, 2402 30g of phenolic resin, 5g of single-walled carbon nanotube, 5g of graphite powder, 10g of zinc oxide whisker, AO-2246 10g and N330 15g.
The preparation process is the same as in example 1.
Example 3
The embodiment provides a composite rubber material, which specifically comprises the following components:
75g of brominated butyl rubber, 8.33g of polynorbornene rubber, 16.67g of ethylene propylene diene monomer, 10g of zinc oxide, 3g of stearic acid, 2g of magnesium oxide, 2g of sulfur, 2g of BZ, 3g of CZ, 3g of DCP, 1g of TMTD, 3g of DMDT, 2402 30g of phenolic resin, 5g of single-walled carbon nanotube, 10g of graphite powder, AO-2246, 10g of N330, and 15g of the single-walled carbon nanotube.
The preparation process is the same as in example 1.
Example 4
The embodiment provides a composite rubber material, which specifically comprises the following components:
75g of brominated butyl rubber, 16.67g of polynorbornene rubber, 8.33g of ethylene propylene diene monomer, 10g of zinc oxide, 3g of stearic acid, 2g of magnesium oxide, 2g of sulfur, 2g of BZ, 3g of CZ, 3g of DCP, 1g of TMTD, 3g of DMDT, 2402 30g of phenolic resin, 5g of single-walled carbon nanotube, 10g of graphite powder, AO-2246, 10g of N330, and 15g of the single-walled carbon nanotube.
The preparation process is the same as in example 1.
Comparative example 1
The comparative example provides a composite rubber material, which specifically comprises the following components:
100g of brominated butyl rubber, 10g of zinc oxide, 3g of stearic acid, 2g of magnesium oxide, 2g of sulfur, 2g of BZ, 3g of CZ, 3g of DCP, 1g of TMTD, 3g of DMDT, 2402, 0g of phenolic resin and N330.
The preparation process comprises the following steps:
(1) The brominated butyl rubber and the damping agent phenolic resin are firstly added into an internal mixer for mixing for 2min at the mixing temperature of 100 ℃, so that the phenolic resin is completely softened and uniformly dispersed in a rubber matrix.
(2) Then adding the uniformly premixed zinc oxide, stearic acid and magnesium oxide for banburying for 2min.
(3) And then adding a reinforcing filler for banburying for 8min to uniformly disperse the reinforcing filler in the rubber matrix material, and stopping cooling after the rubber is observed to be completely eaten.
(4) Cooling to about 70 ℃, adding a vulcanizing agent, a peroxide crosslinking agent and an accelerant which are mixed uniformly in advance, and banburying for 2min to uniformly disperse various auxiliaries in the rubber matrix material.
(5) And (4) sheet discharging is carried out on an open mill with the roller spacing kept at 2mm, and the master batch is obtained after cooling.
(6) And (3) standing the master batch for 24h, and then putting the master batch into a vulcanizing machine to vulcanize for 30min at 150 ℃.
Comparative example 2
This comparative example provides a compounded rubber material, the specific composition of which differs only from example 1:
the polynorbornene rubber is replaced by nitrile rubber.
The preparation process is the same as in example 1.
Test examples
The properties of the composite rubber materials prepared in the above examples and comparative examples were tested. The results are shown in Table 1.
TABLE 1
The data in the table show that the wide-temperature-range high-damping composite rubber material prepared by the invention can simultaneously improve the basic mechanical property, damping property and bonding property of rubber materials, and the preparation process is simple. The mechanical properties of the rubber prepared by the invention are basically kept consistent, the damping performance at normal temperature and high temperature is obviously improved, the peak value of the damping peak is improved and moves towards the high temperature direction, the effective damping temperature range of tan delta more than or equal to 0.4 is obviously widened, and meanwhile, the bonding strength of rubber and a metal material is obviously improved.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. A composite rubber material, comprising: raw rubber and a damping agent with the weight ratio of 2.5-5;
the raw rubber consists of butyl rubber, polynorbornene rubber and ethylene propylene diene monomer rubber;
the weight percentage of the ethylene propylene diene monomer in the raw rubber is 8-20%;
the damping agent is at least one of terpene resin or modified terpene resin.
2. The composite rubber material according to claim 1, wherein the butyl rubber is 65 to 75% by weight of the raw rubber.
3. The composite rubber material according to claim 1 or 2, wherein the weight ratio of the butyl rubber, the polynorbornene rubber and the ethylene propylene diene rubber is 3-9.
4. The composite rubber material according to any one of claims 1 to 3, wherein the modified terpene resin is at least one of a phenol-aldehyde modified terpene resin, a phenol-modified terpene resin, and an aromatic hydrocarbon modified terpene resin.
5. The composite rubber material according to any one of claims 1 to 4, wherein the butyl rubber is a chlorinated butyl rubber and/or a brominated butyl rubber.
6. The composite rubber material according to any one of claims 1 to 5, further comprising: a reinforcing filler;
the reinforcing filler is at least one of graphene, graphene oxide, graphite powder, single-arm or multi-arm carbon nano tubes, AO-2246, fumed silica, flaky mica powder, kaolin, argil and montmorillonite;
the weight ratio of the reinforcing filler to the raw rubber is 1;
preferably, the weight ratio of the reinforcing filler to the butyl rubber, the polynorbornene rubber and the ethylene propylene diene monomer is 2-5: 3 to 9:0.4 to 4:1.
7. the composite rubber material according to any one of claims 1 to 6, characterized in that it comprises the following components in parts by weight:
100 portions of crude rubber, 20 to 40 portions of damping agent, 3 to 10 portions of zinc oxide, 1 to 3 portions of stearic acid, 0.5 to 2 portions of magnesium oxide, 40 to 80 portions of reinforcing filler, 1 to 5 portions of vulcanizing agent and 4 to 10 portions of accelerant.
8. The compounded rubber material according to claim 7, characterized in that it comprises the following components in parts by weight:
65-75 parts of butyl rubber, 8-20 parts of polynorbornene rubber, 8-20 parts of ethylene propylene diene monomer, 20-40 parts of damping agent, 3-10 parts of zinc oxide, 1-3 parts of stearic acid, 0.5-2 parts of magnesium oxide, 40-50 parts of reinforcing filler, 1-5 parts of vulcanizing agent and 4-10 parts of accelerator.
9. A process for producing a composite rubber material according to any one of claims 1 to 8, characterized by comprising:
(1) Plasticating the raw rubber at 50-80 ℃;
(2) Mixing the plasticated raw rubber with other components, and then banburying at a temperature higher than the softening point of the damping agent;
(3) Carrying out thin passing, triangular packaging and discharging on the rubber composite material subjected to banburying;
(4) And vulcanizing the discharged rubber composite material at the temperature of 140-170 ℃ to obtain the rubber composite material.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11198269A (en) * | 1998-01-16 | 1999-07-27 | Bando Chem Ind Ltd | Seismic isolation structure and its manufacture |
| JP2005089727A (en) * | 2003-08-11 | 2005-04-07 | Du Pont Mitsui Polychem Co Ltd | Vulcanized rubber composition |
| CN101418109A (en) * | 2007-10-23 | 2009-04-29 | 上海华向橡胶制品有限公司 | High temperature and high damping resistant rubber composite using polynorbornene rubber as main body |
| CN109320861A (en) * | 2018-10-25 | 2019-02-12 | 株洲时代新材料科技股份有限公司 | A kind of wide temperature zone high damping halogenated butyl rubber material and preparation method thereof |
| CN111675859A (en) * | 2020-06-28 | 2020-09-18 | 天津东丰和美新材料科技有限公司 | Damping material and preparation method thereof |
| CN112266540A (en) * | 2020-10-29 | 2021-01-26 | 新力紧科技(深圳)有限公司 | Low-modulus ultrahigh-damping elastic material for building rubber support |
-
2022
- 2022-10-28 CN CN202211338346.3A patent/CN115651324A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11198269A (en) * | 1998-01-16 | 1999-07-27 | Bando Chem Ind Ltd | Seismic isolation structure and its manufacture |
| JP2005089727A (en) * | 2003-08-11 | 2005-04-07 | Du Pont Mitsui Polychem Co Ltd | Vulcanized rubber composition |
| CN101418109A (en) * | 2007-10-23 | 2009-04-29 | 上海华向橡胶制品有限公司 | High temperature and high damping resistant rubber composite using polynorbornene rubber as main body |
| CN109320861A (en) * | 2018-10-25 | 2019-02-12 | 株洲时代新材料科技股份有限公司 | A kind of wide temperature zone high damping halogenated butyl rubber material and preparation method thereof |
| CN111675859A (en) * | 2020-06-28 | 2020-09-18 | 天津东丰和美新材料科技有限公司 | Damping material and preparation method thereof |
| CN112266540A (en) * | 2020-10-29 | 2021-01-26 | 新力紧科技(深圳)有限公司 | Low-modulus ultrahigh-damping elastic material for building rubber support |
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