CN109320964A - A kind of phenyl siloxane rubber sponge damping material and preparation method thereof - Google Patents
A kind of phenyl siloxane rubber sponge damping material and preparation method thereof Download PDFInfo
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- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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Abstract
The invention discloses a kind of phenyl siloxane rubber sponge damping material and preparation method thereof, raw material includes: 100 parts of phenyl siloxane rubber, 30~60 parts of white carbon black, 0.5~2 part of vulcanizing agent, 1~15 part of blowing agent H, 0.5~10 part of blowing promotor according to weight fraction meter.The method for introducing foam structure in phenyl siloxane rubber matrix using chemical foaming technology, is prepared for the phenyl siloxane rubber damping material with wide temperature range damping characteristic.The phenyl siloxane rubber sponge abscess of this method preparation is fine and closely woven, and uniformity is good, has wide temperature range damping characteristic, suitable for preparing damping shock absorption, heat-insulated, insulating element, uses in fields such as aerospace, communications and transportation, instrument, daily lifes.
Description
Technical field
The present invention relates to technical field of polymer material processing, and in particular to a kind of phenyl siloxane rubber sponge damping material and
Preparation method.
Background technique
The physical significance of damping is the decaying of power, or the energy dissipation of object during exercise.When object is by external force
And when vibrating, a kind of counter-force for making external force decay, referred to as damping force or damping force can be generated.The ratio of it and active force, which is referred to as, to be hindered
Buddhist nun's coefficient.The direction of usual damping force is always opposite with the directional velocity of movement.Therefore, the damped coefficient of material is bigger, meaning
Its damping effect or damping it is better.Rubber is a kind of highly desirable damping material, this is because rubber is macromolecular material
Material, molecular volume is huge, leads to violent interior friction under external force, produces reaction force.This power is external in resistance
During vibration, the amplitude of vibration is on the one hand weakened, is on the other hand converted into thermal energy from mechanical energy again, realized energy and turn
It changes.Various anti-vibration articles can be made in material based on rubber, such as subtracting on machine, engine, vehicle, naval vessel, aircraft
Shake part etc..Yielding rubber is also widely used in the vehicles, such as matched damping part on locomotive, automobile, rail resilient cushion, bridge
Beam support etc..Visco-elastic damping material and its product designing technique are widely used to various rockets, guided missile, satellite, army at present
With and civil aircraft, naval vessel and vehicle on instrument and meter, navigation equipment and electronic system etc. vibration control and noise control
[1] (Zhao Yunfeng, aerospace material technique, 2009, No.5, pp.1-6), it has also become essential key in Aerospace Engineering
One of technology.
Ideal damping material requires have the high-damping factor within the scope of wide temperature range, it is made to have better environment to adapt to
Property, it is suitable for more conglomerate.The shortcomings that rubber elastomer damping material, is the glass transition region temperature of single rubber clone
Range is generally all relatively narrow, and only 20~40 DEG C, and all room temperature is concentrated on hereinafter, therefore damping function area temperature range is narrow and uses
Temperature is relatively low, and damping capacity more than room temperature is bad, it is difficult to meet the needs of practical engineering application.
The special backbone structure of silicon rubber makes it have excellent high and low temperature resistance, while in wider temperature range
(- 50 DEG C~200 DEG C) mechanical property and damping capacity are stablized.It is general viscous that the stability of this performance is different from silicon rubber
Elastic material becomes the first choice of the fields such as aerospace, precision instrument damping material.But silicon rubber is in -50 DEG C~150 DEG C models
Its fissipation factor tan δ is lower in enclosing, and about 0.05~0.1, it is not able to satisfy actual operation requirements [2] (Huang Yanhua, Shi Yang, Xue Lei
Deng aeronautical material journal, 2016, Vol.36, No.3, pp.79-91).
Side-chain radical can be changed by block copolymerization at present, be blended with other organic polymers or interpenetrating polymer net
The modes such as network, and addition damping additive can further improve the damping of silicon rubber.These methods can improve in various degree
The damping capacity of silicon rubber, but have respective deficiency.Change side-chain radical by block copolymerization and interpenetrating networks promote silicon rubber
Glue damping performance methodology is still in the laboratory research stage, is difficult to industrialized production at present.By being blended with high-damping polymer
It is to improve the convenient method of silicon rubber damping, but the composition of material can be changed, reduces the characteristics such as the high-low temperature resistant of silicon rubber.Add
Add small molecule damping agent method that can also change material composition, and small molecule migration occurs in use process and influences damping material
The stability of performance.
It is the new skill for preparing silicon rubber damping material by introducing foam structure come the damping capacity for improving silicone rubber matrix
Art approach.The method of vinylsiloxane rubber foaming at present has two classes.One kind is the method for chemical blowing, usually utilizes chemistry hair
The gas that infusion thermal degradation releases forms bubble.This foaming method is suitable for making the foamed material of hole-closing structure.By
In in process, vulcanization carries out simultaneously with two chemical processes of foaming, and the matching of sulfidation and foaming process is to prepare
The key of foam structure and the sponge material of function admirable.But common peroxide vulcanizing agent and foaming agent are equal to temperature
Very sensitive, temperature is every to increase 10 DEG C, and curingprocess rate and foaming agent decomposition rate are multiplied, in addition, peroxide cure
Agent decomposes the influence of residue vulnerable to foaming agent and reduces the cross-linking efficiency of peroxide, in order to adjust the crosslinking speed of peroxide
Degree, it is often necessary to add and formula and technical study is repeated, it is therefore, this to reach the matching of crosslinking rate and expansion rate
The implementation of method and control difficulty are larger.Another kind of foaming method is Physical Foaming method: using Inert particulate pore former and silicon rubber
After glue mixing, the pore-forming by the methods of dissolved removal inertia pore former obtains the silicone sponge material of open-celled structure.But
It is that this foaming method efficiency is lower, energy consumption is high, needs to consume a large amount of inertia pore former, in addition, a large amount of particulate pore formers exists
It is not only difficult to be uniformly dispersed in rubber matrix, but also influences the process industrial art performance of rubber.
The phenyl that large volume is introduced in silicon rubber molecular side chain is conducive to improve the energy consumption of silicon rubber molecular chain movement
It dissipates, to improve the damping capacity of silicon rubber.But the phenyl of large volume is introduced on silicon rubber molecular side chain, change silicon rubber
The Nomenclature Composition and Structure of Complexes of xanthan molecule chain affects the flexibility of silicon rubber strand and the active force of molecule interchain.It was found that,
The high phenyl siloxane rubber of phenyl content 30mol% shows apparent roll banding phenomenon in mixing process, shows a large amount of phenyl
Introducing makes silicon rubber processing performance that significant change have occurred.
Summary of the invention
The purpose of the present invention is provide a kind of phenyl siloxane rubber sponge damping material and its system in view of the drawbacks of the prior art
Preparation Method uses the phenyl siloxane of higher molecular weight as basis material, and filling white carbon black enhances matrix, root
According to sulfur foam system registration property, in conjunction with segmentation chemical foaming technology, thus the phenyl siloxane rubber of the hole-closing structure prepared is extra large
Continuous abscess is fine and closely woven, and uniformity is good, suitable for preparing damping shock absorption, sound insulation, heat-insulated, insulating element.
In order to reach above-mentioned technical effect, the present invention provides a kind of phenyl siloxane rubber sponge damping material, raw material is pressed
It include: 100 parts of phenyl siloxane rubber according to weight fraction meter, 30~60 parts of white carbon black, 0.5~2 part of vulcanizing agent, blowing agent H 1~15
Part, 0.5~10 part of blowing promotor.
Further technical solution is that wherein phenyl content is not less than 5%mol, and the white carbon black is selected from surface hydrophobic
White carbon black, the blowing promotor are the mixture of zinc oxide, urea or both.
Further technical solution is that the vulcanizing agent is selected from vulcanizing agent DCP or bis 25 vulcanizing agent.
The present invention also provides a kind of preparation methods of phenyl siloxane rubber sponge damping material, comprising the following steps:
(1) phenyl siloxane rubber and white carbon black will be entered into mixer and will be carried out high temperature mixing 10~20 minutes, then parked
24 hours, obtain phenyl siloxane rubber composition；
(2) phenyl siloxane rubber composition, blowing agent H and blowing promotor are added in mixer, 2~5 is kneaded under room temperature
Minute, vulcanizing agent is then added and continues mixing 3~7 minutes, parks 12 hours, obtains silicone sponge composition；
(3) silicone sponge is put into mold with composition and carries out presulfurization foaming, then increase temperature
Afterwards, post-cure molding is being carried out, is obtaining phenyl siloxane rubber sponge damping material.
Further technical solution is that the temperature of step (1) the high temperature mixing is 90 DEG C~120 DEG C.
Further technical solution is that the temperature that room temperature is kneaded in the step (2) is 15 DEG C~40 DEG C.
Further technical solution is, in the step (3) presulfurization and temperature is 120 DEG C~145 DEG C, once
Prevulcanisation time is 25~30 minutes.
Further technical solution is that the temperature of post-cure is 160 DEG C~180 DEG C in the step (3), post-cure
Time be 15~25 minutes.
The present invention is further explained and is illustrated below, the present invention is using chemical foaming technology in phenyl siloxane rubber
The method that specific foam structure is introduced in matrix is prepared for the phenyl siloxane rubber sponge damping material with wide temperature range damping characteristic
Material.Based on interfacial damping and air damping principle, using phenyl siloxane rubber as matrix, designed using matched foam structure, substantially
Degree amplification matrix damping characteristic, obtains the elastomer for having both wide temperature range damping characteristic.Hole-closing structure silicone sponge is in silicon rubber
A large amount of gas-solid interface is formed in matrix, the accumulation of the air damping effect in interfacial damping effect and abscess significantly mentions
The damping capacity of silicone rubber matrix is risen.In addition, the molecular structure feature of the phenyl siloxane rubber used is on polysiloxane chain side
With phenyl group.Phenyl siloxane rubber not only has the performance characteristics of methyl vinyl silicone rubber, but also due in molecular side chain
The phenyl for introducing large volume is modified, and improves molecule chain rigidity, increases the energy dissipation of molecular chain movement, favorably
In the damping capacity for improving silicon rubber.In addition, be substituted by phenyl due to the methyl moiety that is connected on this kind of strand side with silicon,
So the regularity of chain is destroyed, so as to improve the cryogenic property of polymer.Phenyl siloxane rubber has further widened silicon rubber
Use scope, can satisfy the industries such as Aeronautics and Astronautics to it is low temperature resistant and radiation harsh environment requirement.
Using phenyl siloxane rubber as matrix, using hydrophabic silica as reinforcing agent, organic foaming agent and peroxide sulphur
The foaming vulcanizing system that agent matches, hot press moulding moulding process prepare silicone sponge damping material.Organic foaming agent exists
Generation gas is decomposed under high temperature makes sizing material foam, and when the expansion rate of sizing material matches with rate of cure, passes through hot press moulding
Moulding process can prepare the hole-closing structure phenyl siloxane rubber sponge material of different apparent density.
By using blowing promotor in formula, the thermal decomposition temperature and rate of foaming agent are had adjusted, phenyl siloxane rubber is made
The expansion rate and rate of cure of sizing material match, in molding vulcanization process, in order to obtain the sponge material of hole-closing structure
Material, sizing material divide post vulcanization, first use relatively low curing temperature, and the foaming of sizing material is made to carry out a degree of base in vulcanization
Occur on plinth, at this point, sizing material has certain intensity because being tentatively crosslinked, foaming agent can be encased and decompose the gas generated, together
When because crosslinking degree it is low, sizing material has certain plasticity again, can deform with the increase of gas.With the increasing of expansion rate
Add, bubble is constantly grown up；Meanwhile the increase of rate of cure increases the crosslinking degree of sizing material constantly, until gas pressure in sizing material
Power and vulcanized network balance each other to the restraining force of rubber deformation, and the gas that foaming agent thermally decomposes to generate is synchronizing the glue being crosslinked
Abscess is formed in material；It carries out sulfidization molding at a higher temperature again, obtains the phenyl siloxane rubber sponge of hole-closing structure.Pass through
White carbon black is added in sizing material, not only improves the plasticity of sizing material, and improves the mechanical property of silicone sponge.These
Particle may be uniformly dispersed in sizing material, play the role of nucleating agent, keep the abscess of sizing material more uniform.
The present invention has the advantages that, the phenyl siloxane rubber sponge damping material of this method preparation due to use compared with
The phenyl siloxane of high molecular weight is basis material, and filling white carbon black enhances matrix, thus the closed pore knot prepared
The phenyl siloxane rubber sponge abscess of structure is fine and closely woven, and uniformity is good, suitable for preparing damping shock absorption, sound insulation, heat-insulated, insulating element,
The fields such as aerospace, communications and transportation, petrochemical industry, instrument, style and daily life use.In addition, this method uses high temperature
Vulcanization compression molding technology prepares phenyl siloxane rubber sponge damping material, can be in open mill, mixer, vulcanizing press
Etc. implement in common rubber processings equipment, without purchasing special process equipment, have that small investment, technological operation be easy, production effect
Rate height, advantage at low cost.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of phenyl siloxane rubber sponge damping material prepared by the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of phenyl siloxane rubber sponge damping material prepared by the embodiment of the present invention 2；
Fig. 3 is the scanning electron microscope (SEM) photograph of phenyl siloxane rubber sponge damping material prepared by the embodiment of the present invention 3；
Fig. 4 is the scanning electron microscope (SEM) photograph of phenyl siloxane rubber sponge damping material prepared by the embodiment of the present invention 4；
Fig. 5 is the scanning electron microscope (SEM) photograph of the phenyl siloxane rubber damping material of reference examples 2 of the present invention preparation；
Specific embodiment
Below with reference to the embodiment of the present invention, the invention will be further elaborated.
Embodiment 1
100 parts of phenyl siloxane rubbers (phenyl content 30mol%) are added in mixing chamber, are divided with 40 parts of white carbon black mixings 15
Clock obtains phenyl siloxane rubber composition, is added 10 parts of blowing promotor, 15 parts of foaming agent, is kneaded 3 minutes, vulcanizing agent is then added
1.2 parts, it is kneaded 5Min, obtains phenyl siloxane rubber sponge damping material composition；
It is respectively 100mm × 100mm × 10mm that 70g silicone sponge, which is put into die cavity length, width and height with damping material composition,
Mold in, after 120 DEG C of presulfurizations next time are foamed 30 minutes, be warming up to post-cure 20 minutes at 160 DEG C, obtain phenyl
Silicone sponge damping material.It is tested for the property, test result such as table 2 and table 3.
Embodiment 2
Unlike the first embodiment, 10 parts of foaming agent, 5 parts of blowing promotor, 1.0 parts of vulcanizing agent, silicone sponge damping
Material compositions loading is 80g, remaining process conditions and operating procedure with embodiment 1, and the formula of silicone sponge is shown in Table 1,
Performance is shown in Table 2 and table 3.
Embodiment 3
Unlike the first embodiment, 5 parts of foaming agent, 3 parts of blowing promotor, 1.5 parts of vulcanizing agent, silicon rubber sponge composite
Loading is 90g, remaining process conditions and operating procedure are with embodiment 1, and the formula of silicone sponge is shown in Table 1, and performance is shown in Table 2 Hes
Table 3.
Embodiment 4
Unlike the first embodiment, pre-curing temperature is 145 DEG C, foamed time 25 minutes, remaining process conditions and
Operating procedure is with embodiment 1, and the formula of silicone sponge is shown in Table 1, and performance is shown in Table 2 and table 3.
Reference examples 1
Foaming agent and auxiliary agent is not added with embodiment 1 in operation.100 parts of phenyl siloxane rubbers are added in mixing chamber white with 40 parts
Carbon black mixing 15 minutes, obtain phenyl siloxane rubber composition.At room temperature, it is added vulcanizing agent DCP1.2 parts, is kneaded 7 minutes, obtains
Obtain silicon rubber composition.
25g silicon rubber, which is put into die cavity length, width and height with composition, is respectively in 100mm × 100mm × 2mm mold,
160 DEG C vulcanize 20 minutes next time, obtain silastic material.The formula of phenyl siloxane rubber material is shown in Table 1, and performance is shown in Table 2 and table
3。
Reference examples 2
Unlike the first embodiment use a sulfidization molding, 160 DEG C of curing temperature, the time 15 minutes, remaining technique item
Part and operating procedure are with embodiment 1, and the formula of silicone sponge is shown in Table 1, and performance is shown in Table 2 and table 3.
The formula of 1 phenyl siloxane rubber sponge damping material of table
| Phenyl siloxane rubber | White carbon black | Vulcanizing agent DCP | Blowing agent H | Blowing promotor | |
| Embodiment 1 | 100 | 40 | 1.2 | 15 | 10 |
| Embodiment 2 | 100 | 40 | 1.0 | 10 | 5 |
| Embodiment 3 | 100 | 40 | 1.5 | 5 | 3 |
| Embodiment 4 | 100 | 40 | 1.2 | 15 | 10 |
| Reference examples 1 | 100 | 40 | 1.2 | — | — |
| Reference examples 2 | 100 | 40 | 1.2 | 15 | 10 |
Draftability is carried out respectively to phenyl siloxane rubber sponge damping material prepared by Examples 1 to 4 and reference examples 1~2
The test of energy, test result are as shown in table 2.
The tensile property of 2 phenyl siloxane rubber sponge damping material of table
As can be seen from Table 2, compared with unexpanded phenyl siloxane rubber (reference examples 1), foaming phenyl siloxane rubber density compared with
It is low, tensile property decline；Compared with reference examples 2, have by phenyl siloxane rubber sponge prepared by step up cure foam process thin
Close foam structure, higher tensile strength, elongation at break and 100% stress at definite elongation.
Damping and amortization is carried out respectively to phenyl siloxane rubber sponge damping material prepared by Examples 1 to 4 and reference examples 1~2
The test of energy, test result are as shown in table 3.
The damping capacity of 3 phenyl siloxane rubber sponge damping material of table
In table 3, Tg indicates glass transition temperature, tan δmaxIndicate maximum loss factor, △ T(tanδ≥0.2)Indicate loss
The factor is greater than or equal to 0.2 damping temperature domain.
As can be seen from Table 3, compared with unexpanded silicon rubber (reference examples 1), the glass transition for the phenyl siloxane rubber that foams
Temperature Tg is reduced, storage modulus E ' reduction, and fissipation factor tan δ is increased.With the molding phenyl siloxane rubber sponge of a sulfur foam
(reference examples 2) are compared, and the phenyl siloxane rubber sponge glass transition temperature of Examples 1 to 4 preparation is lower, tan δmaxWith loss because
Sub- tan δ is higher, and the fissipation factor tan δ of low temperature and room temperature area near -50 DEG C~30 DEG C, phenyl siloxane rubber sponge is greater than
0.3, in -50 DEG C~100 DEG C temperature ranges, fissipation factor tan δ is greater than or equal to 0.2, phenyl silicon rubber prepared by embodiment 4
Temperature range of the gelatin sponge fissipation factor tan δ more than or equal to 0.2 reaches 200 DEG C, has good damping and amortization in wide temperature range
Can, suitable for the damping material to industries such as the demanding aerospaces of environmental adaptability.
Claims (8)
1. a kind of phenyl siloxane rubber sponge damping material, which is characterized in that its raw material includes: phenyl silicon rubber according to weight fraction meter
100 parts of glue, 30~60 parts of white carbon black, 0.5~2 part of vulcanizing agent, 1~15 part of blowing agent H, 0.5~10 part of blowing promotor.
2. phenyl siloxane rubber sponge damping material according to claim 1, which is characterized in that the phenyl siloxane rubber is selected from
Methyl vinyl phenyl silicon rubber, wherein phenyl content is not less than 5%mol, and the white carbon black is selected from surface hydrophobic white carbon black,
The blowing promotor is the mixture of zinc oxide, urea or both.
3. phenyl siloxane rubber sponge damping material according to claim 1, which is characterized in that the vulcanizing agent is selected from vulcanization
Agent DCP or bis 25 vulcanizing agent.
4. a kind of preparation method of phenyl siloxane rubber sponge damping material, which comprises the following steps:
(1) phenyl siloxane rubber and white carbon black will be entered into mixer and will be carried out high temperature mixing 10~20 minutes, it is small then to park 24
When, obtain phenyl siloxane rubber composition；
(2) phenyl siloxane rubber composition, blowing agent H and blowing promotor are added in mixer, are kneaded 2~5 minutes under room temperature,
Then vulcanizing agent is added and continues mixing 3~7 minutes, parks 12 hours, obtains silicone sponge composition；
(3) silicone sponge is put into mold with composition and carries out presulfurization foaming, after then increasing temperature,
Post-cure molding is carried out, phenyl siloxane rubber sponge damping material is obtained.
5. the preparation method of phenyl siloxane rubber sponge damping material according to claim 4, which is characterized in that the step
(1) temperature of high temperature mixing is 90 DEG C~120 DEG C.
6. the preparation method of phenyl siloxane rubber sponge damping material according to claim 4, which is characterized in that the step
(2) temperature that room temperature is kneaded in is 15 DEG C~40 DEG C.
7. the preparation method of phenyl siloxane rubber sponge damping material according to claim 4, which is characterized in that the step
(3) in a presulfurization and temperature is 120 DEG C~145 DEG C, prevulcanisation time is 25~30 minutes.
8. the preparation method of phenyl siloxane rubber sponge damping material according to claim 4, which is characterized in that the step
(3) temperature of post-cure is 160 DEG C~180 DEG C in, and the time of post-cure is 15~25 minutes.
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| CN113388251A (en) * | 2020-03-11 | 2021-09-14 | 中国石油化工股份有限公司 | Rubber composition based on low-phenyl silicone rubber, vulcanized rubber, and preparation method and application thereof |
| CN113388252A (en) * | 2020-03-11 | 2021-09-14 | 中国石油化工股份有限公司 | Rubber composition, vulcanized rubber, and preparation method and application thereof |
| CN113388251B (en) * | 2020-03-11 | 2022-09-20 | 中国石油化工股份有限公司 | Rubber composition based on low-phenyl silicone rubber, vulcanized rubber, and preparation method and application thereof |
| CN113388252B (en) * | 2020-03-11 | 2022-09-20 | 中国石油化工股份有限公司 | Rubber composition, vulcanized rubber, and preparation method and application thereof |
| CN113644779A (en) * | 2021-07-15 | 2021-11-12 | 浙江零跑科技股份有限公司 | New forms of energy car damping vibration isolation noise reduction device |
| CN113644779B (en) * | 2021-07-15 | 2022-07-19 | 浙江零跑科技股份有限公司 | New forms of energy car damping vibration isolation noise reduction device |
| CN115819980A (en) * | 2022-12-05 | 2023-03-21 | 广东电网有限责任公司 | Environment-friendly flame-retardant foamed silicone rubber and preparation method and application thereof |
| CN115819980B (en) * | 2022-12-05 | 2024-01-26 | 广东电网有限责任公司 | Environment-friendly flame-retardant foam silicone rubber and preparation method and application thereof |
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