CN107698916B - Wide temperature range acrylic rubber base graphene oxide damping material and preparation method thereof - Google Patents
Wide temperature range acrylic rubber base graphene oxide damping material and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/13—Phenols; Phenolates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/18—Amines; Quaternary ammonium compounds with aromatically bound amino groups
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- C08K5/00—Use of organic ingredients
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- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
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Abstract
The invention discloses a kind of wide temperature range acrylic rubber base graphene oxide damping materials and preparation method thereof.It the steps include: to prepare certain size, surface has the graphene oxide dispersion of a large amount of polar groups by adjusting oxidizer；ACM is mixed with the various compounding agents such as hindered phenol small molecule, vulcanizing agent using mechanical blending method, is then mixed using solution blended process with graphene oxide, the ACM base damping rubber of the wide temperature range of the invention containing graphene oxide can be obtained in dry, vulcanization.The present invention forms strong hydrogen bond using between graphene oxide, hindered phenol small molecule and ACM of the surface with a large amount of polar groups, the barrier property of graphene oxide, the effective damping temperature range (δ >=0.3 tan) for substantially increasing ACM base graphene oxide damping material and its damping capacity after aging are utilized simultaneously.
Description
Technical field
The invention belongs to the technical fields of damping material preparation, and in particular to a kind of width temperature range acrylic rubber (ACM)
Base graphene oxide damping material and preparation method thereof.
Background technique
With the development of contemporary industry technology, every field gradually realizes the mechanization and automation of production.Although this
Bring great convenience to our production and life, but its adjoint vibration and noise also give we health and
Mental health brings great hidden danger, while vibration can also seriously affect the service life for influencing mechanical equipment, improves equipment
Maintenance cost.So damping noise reduction becomes current urgent problem.It the use of damping material is the master for solving the problems, such as this
Want one of means.Vibrational energy harmony can be largely changed into the material that thermal energy consumption dissipates as a kind of by visco-elastic damping material,
It is a kind of excellent damping damping material.
Currently, in visco-elastic damping material research field, the main problems are as follows: (1) visco-elastic damping material
Good damping capacity is mainly near glass transition temperature, but lower glass transition temperature is (most of subzero
Degree Celsius) for actual condition, application value is not high；(2) visco-elastic damping material tends not to take into account high damping and amortization
It can (fissipation factor tanδ>=0.3) and wide effective damping temperature range (tanδ>=0.3 temperature range) two conditions；(3) it hinders
Buddhist nun's process is the process that kinetic energy is converted into thermal energy, therefore in actual use, rubber internal heat steeply rises, on the one hand
It is easy to cause the migration of small molecule damping agent to be lost, loses damping, on the other hand lead to the aging of rubber molecular chain.Cause
How this, solve the above problems simultaneously, be to prepare one of research hotspot of damping rubber.
Summary of the invention
The object of the present invention is to provide one kind to have the wide temperature range of high-damping, still with the resistance of preferable damping capacity after aging
Damping material and preparation method thereof.
Realize that technical solution of the invention is as follows:
The wide temperature range acrylic rubber base graphene oxide damping material includes acrylate in terms of mass parts
100 parts of rubber, 20~60 parts of hindered phenol small molecule, 0.1~0.5 part of graphene oxide, 1~3 part of stearic acid, vulcanization accelerator 1
~6 parts, 2~5 parts of anti-aging agent, 2~4 parts of processing aid, 1~4 part of vulcanizing agent.
Wherein, the hindered phenol small molecule is any one in AO-60 and AO-80 or two kinds.
The vulcanization accelerator is any one in 1,3- diphenylguanidine (D) and 1,3- bis--o- tolyl guanidine (DOTG)
Or two kinds.
The anti-aging agent is N- isopropyl-N'- diphenyl-para-phenylene diamine (4010NA) and N, N'- diphenyl-para-phenylene diamine
(DPPD) any one in or two kinds.
The processing aid is any one or a few in RL210, WS280 and WB222.
The vulcanizing agent is Sulfur.
The preparation method of the acrylate-based graphene oxide damping material of above-mentioned width temperature range, comprising the following steps:
Step 1, large scale, high oxidation degree graphene oxide are prepared using improved Hummers method, wherein prepared
The mass ratio of Cheng Zhong, potassium permanganate and graphite is 1:1~3:1.
Step 2, graphene oxide ultrasonic disperse step 1 obtained is in water and dimethyl sulfoxide mixed solution, decompression
Distillation is until obtain the dimethyl sulphoxide solution of graphene oxide；
Step 3, by acrylic rubber and hindered phenol small molecule, stearic acid, vulcanization accelerator, anti-aging agent, processing aid
It is kneaded with vulcanizing agent, then thin pass-out piece；It is cooling, it is ground into fine particle, is then dissolved in dimethyl sulphoxide solution；
Step 4, solution blending step 2 and step 3 obtained after dry, vulcanize and wide temperature range ACM base graphite oxide is made
Alkene damping material.
Further, in step 2, the volume ratio of water and dimethyl sulfoxide is 1:1 in water and dimethyl sulfoxide mixed solution,
4~6mg/mL of concentration of the dimethyl sulphoxide solution of graphene oxide.
Compared with prior art, the present invention its remarkable advantage is:
(1) present invention obtains large scale, single layer and surface with largely containing by adjusting the ratio of potassium permanganate and graphite
The graphene oxide of oxygen groups can uniformly be mixed graphene oxide and ACM using solution blending；Stone is aoxidized using large scale
Constraint of the black alkene to the strand of rubber improves the glass transition temperature of rubber material.
(2) present invention using specific promotor 1,3- diphenylguanidine (D) and/or 1,3- bis--o- tolyl guanidine (DOTG) and
Interaction between graphene oxide, hindered phenol small molecule is formed strong between graphene oxide, hindered phenol and its ACM
Hydrogen bond action, using the barrier action of large-sized graphene oxide and its hydrogen bond action between hindered phenol, prevent by
Hinder the migration in rubber at high temperature of phenol small molecule.Improve damping capacity of the damping material after ageing of rubber.
(3) present invention specific anti-aging agent N- isopropyl-N'- diphenyl-para-phenylene diamine (4010NA) and/or N, N'- hexichol
The weak bond of varying strength closes between base p-phenylenediamine (DPPD) and graphene oxide and small molecule damping agent, i.e., at different temperatures
There is the weak bond of varying strength to close, so that there are enough weak bonds to close in wider temperature range and occur to be broken and be bonded again, from
And widen effective damping temperature range.
(4) when filling 0.5 part of graphene oxide and when 60 parts of AO-80, the effective damping temperature range of material -8.1 DEG C~
38.4 DEG C, temperature range width reaches 46.5 DEG C, and the material temperature range for being relatively not filled by graphene oxide improves 9.4 DEG C, and low temperature and
Damping factor at high temperature is also improved.The damping temperature domain of material can reach 44.2 DEG C after aging, relatively be not filled by oxygen
The material temperature range of graphite alkene improves 25.7 DEG C.
Detailed description of the invention
Fig. 1 is the preparation flow schematic diagram of wide temperature range ACM base graphene oxide damping material prepared by embodiment 1.
Fig. 2 is that the AFM of large scale graphene oxide prepared by embodiment 1 schemes (a) and its corresponding height map (b).
Fig. 3 is the full spectrogram (a) of XPS and its C1s XPS spectrum figure (b) of large scale graphene oxide prepared by embodiment 1.
Fig. 4 be embodiment 1 prepared by wide temperature range ACM base graphene oxide damping material 100 °C lower aging 48 hours
The DMA comparison diagram of front and back.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
The acrylic rubber (ACM rubber) used in following embodiment is commercially available, damping of the trade mark to damping material
Performance has no significant effect.
The present invention mainly uses mechanical blending+solution blending method, remains big ruler of the graphene oxide in rubber
On the one hand very little pattern utilizes large-sized graphene oxide pair by controlling size, single layer and the degree of oxidation of graphene oxide
Effective constraint of rubber molecular chain, improves the glass transition temperature of rubber material；On the other hand surface of graphene oxide is utilized
Active function groups, form the different weak bond of intensity between small molecule damping agent and promotor and close, improve the damping and amortization of rubber
Can, meanwhile, it is further closed using the weak bond of varying strength between anti-aging agent and graphene oxide and small molecule damping agent, i.e., not
There is the weak bond of varying strength to close under synthermal so that in wider temperature range, have enough weak bonds close occur fracture with
It is bonded again, to widen effective damping temperature range；Moreover, large-sized graphene oxide, which can manage it, forms good thermal conducting path
With barrier access, while the heat generated in damping process is dissipated to the external world, it is effectively prevented moving for damping agent small molecule
Move loss.
Embodiment 1
Step 1, the 230 mL concentrated sulfuric acids are measured in four-hole boiling flask, ice bath is down to 0 °C or so.Sequentially add 10 g stones
Ink, 5 g sodium nitrate, 15 min of agitating solution.Then 30 g potassium permanganate are slowly added in three times in 1 h, keep temperature low
In 20 °C.It is warming up to 35 °C after mixing, is kept stirring 2 h.It is slowly added to 460 mL deionized waters later, in this mistake
Cheng Zhong keeps solution temperature to be lower than 100 °C, keeps 15 min, liquid is transferred in beaker, and 750 mL deionized waters are added
With the hydrogenperoxide steam generator of 250 mL 5%.Then graphene oxide is arrived through ultrasound, dialysis, drying and processing, and to graphite oxide
Alkene is characterized, and AFM figure and its corresponding height map are as shown in Fig. 2, XPS figure is as shown in Figure 3；
Step 2, the large-sized graphene oxide of 0.5 g step 1 obtained puts into water and dimethyl sulfoxide mixed solution
In, ultrasound is dispersed in graphene oxide in water mixed solution, and vacuum distillation obtains the graphite oxide that concentration is 5mg/mL
The dimethyl sulphoxide solution of alkene；
Step 3, by 100 parts of ACM rubber, 60 parts of hindered phenol small molecule AO-80,1 part of stearic acid, 1 part of accelerator D, 2
Part antioxidant 4010NA, 2 parts of processing aid RL210, the formula of 1 part of Sulfur are kneaded, then thin pass-out piece.It is cooling, it is ground into thin
Little particle is then dissolved in dimethyl sulphoxide solution；
Step 4, the solution blending that step 2 and step 3 obtain measures its sulfurizing time with vulcameter after dry, according to
Wide temperature range ACM base graphene oxide damping material is made in sulfurizing time vulcanization.
DMA comparison of the wide temperature range ACM base graphene oxide damping material of preparation in 100 °C of lower agings, 48 hours front and backs
Figure is as shown in Figure 4.As a result, it has been found that the effective damping temperature range of obtained damping material is at -8.1 DEG C~38.4 DEG C, temperature range width reaches
46.5 DEG C, the damping temperature domain of material can also reach 44.2 DEG C after aging.
Embodiment 2
1 method of embodiment is repeated, but in step 1, potassium permanganate dosage is 21 g；Graphene oxide is used in step 2
Amount is 0.4 g；In step 3 mixing formula be 100 parts of ACM rubber, 50 parts of hindered phenol small molecule AO-80,3 parts of stearic acid, 2 parts
Accelerator D, 4 parts of accelerator DOTGs, 2 parts of antioxidant 4010NAs, 3 parts of antioxidant DPPDs, 1 part of processing aid RL210,
3 parts of processing aid WS280,4 parts of Sulfurs.The effective damping temperature range of obtained damping material is at -7.2 DEG C~38.0 DEG C, wide temperature range
Degree reaches 45.2 DEG C, and the damping temperature domain of material can also reach 42.4 DEG C after aging.
Embodiment 3
1 method of embodiment is repeated, but in step 1, potassium permanganate dosage is 15 g；Graphene oxide is used in step 2
Amount is 0.3 g；Mixing formula is 100 parts of ACM rubber, 30 parts of hindered phenol small molecule AO-60,2 parts of stearic acid, 2 sulphur in step 3
Change diphenylguanidine OTG, 3 parts of antioxidant DPPDs, 2 parts of processing aid WB222,1 part of processing aid WS280,3 parts of Sulfurs.Obtained resistance
For the effective damping temperature range of damping material at -6.8 DEG C~37.8 DEG C, temperature range width reaches 44.6 DEG C, the damping temp of material after aging
Domain can also reach 42.7 DEG C.
Embodiment 4
1 method of embodiment is repeated, but in step 1, potassium permanganate dosage is 10 g；Graphene oxide is used in step 2
Amount is 0.2 g；Mixing formula is 100 parts of ACM rubber in step 3,10 parts of hindered phenol small molecule AO-80,20 parts small point of hindered phenol
Sub- AO-60,2 parts of stearic acid, 2 accelerator DOTGs, 3 parts of antioxidant DPPDs, 3 parts of processing aid WB222,2 parts of Sulfurs.It obtains
Damping material effective damping temperature range at -7.4 DEG C~37.0 DEG C, temperature range width reaches 44.2 DEG C, the resistance of material after aging
Buddhist nun's temperature range can also reach 43.0 DEG C.
Embodiment 5
1 method of embodiment is repeated, but in step 1, potassium permanganate dosage is 15 g；Graphene oxide is used in step 2
Amount is 0.1 g；Mixing formula is 100 parts of ACM rubber, 20 parts of hindered phenol small molecule AO-80,1 part of stearic acid, 4 sulphur in step 3
Change diphenylguanidine, 3 parts of antioxidant DPPDs, 3 parts of processing aid WS280,4 parts of Sulfurs.The effective damping temperature range of obtained damping material
At -6.4 DEG C~37.5 DEG C, temperature range width reaches 43.9 DEG C, and the damping temperature domain of material can also reach 41.8 DEG C after aging.
Comparative example 1
By the method that specified each component content repeats embodiment 1, but it is free from graphene oxide.As a result, it has been found that obtaining
For the effective damping temperature range of damping material at -4.2 DEG C~32.9 DEG C, temperature range width is 37.1 DEG C, the damping temp of material after aging
Domain drops to 18.5 DEG C.
Comparative example 2
By the method that specified each component content repeats embodiment 1, but directly by the graphene oxide of step 1 preparation
Be kneaded vulcanizing with ACM, AO-80, stearic acid, D, 4010NA, RL210, Sulfur and damping material is prepared.As a result, it has been found that
The effective damping temperature range of damping material is obtained at -4.5 DEG C~33.7 DEG C, temperature range width is 38.2 DEG C, the resistance of material after aging
Buddhist nun's temperature range drops significantly to 25.5 DEG C.
Comparative example 3
By the method that specified each component content repeats embodiment 1, but the dosage of potassium permanganate is 40 g in step 1.
The effective damping temperature range of damping material is obtained at -9.8 DEG C~30.8 DEG C, temperature range width is 40.6 DEG C, the resistance of material after aging
Buddhist nun's temperature range drops significantly to 26.7 DEG C.
Comparative example 4
By the method that specified each component content repeats embodiment 1, but it is free from hindered phenol small molecule.Obtain damping material
Effective damping temperature range at -5.2 DEG C~33.4 DEG C, temperature range width is 38.6 DEG C, under the damping temperature domain of material is significant after aging
Drop to 22.5 DEG C.
Comparative example 5
By the method that specified each component content repeats embodiment 1, but anti-aging agent is 2,2,4- trimethyls -1,2-
Dihyaroquinoline condensate (RD).The effective damping temperature range of damping material is obtained at -5.4 DEG C~30.1 DEG C, temperature range width is
35.5 DEG C, the damping temperature domain of material drops significantly to 29.7 DEG C after aging.
Comparative example 6
By the method that specified each component content repeats embodiment 1, but promotor is N- tert-butyl -2-[4-morpholinodithio
Sulfonamide (NS).The effective damping temperature range of damping material is obtained at -6.8 DEG C~29.3 DEG C, temperature range width is 36.1 DEG C, aging with
The damping temperature domain of material drops significantly to 27.3 DEG C afterwards.
Comparative example 7
By the method that specified each component content repeats embodiment 1, but graphene oxide dosage is 1 g.It is damped
The effective damping temperature range of material is at -10.6 DEG C~29.6 DEG C, and temperature range width is 40.2 DEG C, and the damping temperature domain of material is aobvious after aging
Work drops to 30.5 DEG C.
Claims (6)
1. wide temperature range acrylic rubber base graphene oxide damping material, which is characterized in that include acrylic acid in terms of mass parts
100 parts of ester rubber, 20~60 parts of hindered phenol small molecule, 0.1~0.5 part of graphene oxide, 1~3 part of stearic acid, vulcanization accelerator
1~6 part, 2~5 parts of anti-aging agent, 2~4 parts of processing aid, 1~4 part of vulcanizing agent, wherein
The hindered phenol small molecule is any one or two kinds in AO-60 and AO-80；
The vulcanization accelerator is any one or two kinds in 1,3- diphenylguanidine and 1,3- bis--o- tolyl guanidine；
The anti-aging agent is N- isopropyl-N'- diphenyl-para-phenylene diamine and N, in N'- diphenyl-para-phenylene diamine any one or
Two kinds；
Large scale, high oxidation degree graphene oxide are prepared using improved Hummers method, wherein in preparation process, permanganic acid
The mass ratio of potassium and graphite is 1:1~3:1；
During preparing damping material, by the graphene oxide ultrasonic disperse in water and dimethyl sulfoxide mixed solution,
Vacuum distillation is until obtain the dimethyl sulphoxide solution of graphene oxide.
2. damping material as described in claim 1, which is characterized in that the processing aid is RL210, WS280 and WB222
In any one or a few.
3. damping material as described in claim 1, which is characterized in that the vulcanizing agent is Sulfur.
4. the preparation method of the acrylate-based graphene oxide damping material of width temperature range a method according to any one of claims 1-3,
It is characterized in that, comprising the following steps:
Step 1, large scale, high oxidation degree graphene oxide are prepared using improved Hummers method, wherein in preparation process,
The mass ratio of potassium permanganate and graphite is 1:1~3:1；
Step 2, graphene oxide ultrasonic disperse step 1 obtained is in water and dimethyl sulfoxide mixed solution, vacuum distillation
Until obtaining the dimethyl sulphoxide solution of graphene oxide；
Step 3, by acrylic rubber and hindered phenol small molecule, stearic acid, vulcanization accelerator, anti-aging agent, processing aid and sulphur
Agent is kneaded, then thin pass-out piece；It is cooling, it is ground into fine particle, is then dissolved in dimethyl sulphoxide solution；
Step 4, solution blending step 2 and step 3 obtained after dry, vulcanize and wide temperature range ACM base graphene oxide resistance is made
Damping material.
5. method as claimed in claim 4, which is characterized in that in step 2, water and dimethyl sulfoxide mixed solution Zhong Shui and two
The volume ratio of methyl sulfoxide is 1:1.
6. method as claimed in claim 4, which is characterized in that in step 2, the dimethyl sulphoxide solution of graphene oxide it is dense
Spend 4~6mg/mL.
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| CN108841058A (en) * | 2018-06-01 | 2018-11-20 | 湖南国盛石墨科技有限公司 | A kind of preparation method of high-wearing feature rubber |
| CN110256795B (en) * | 2019-05-17 | 2021-07-27 | 浙江工业大学 | Olefinic carbon damping material with high fireproof performance as well as preparation method and application thereof |
| CN112210216B (en) * | 2020-08-31 | 2022-07-12 | 四川中物材料股份有限公司 | High-damping phenyl silicone rubber and preparation method and application thereof |
| CN112300525B (en) * | 2020-10-27 | 2021-07-23 | 中国科学院金属研究所 | graphene/SEBS composite material with high strength and high damping characteristic and preparation method thereof |
| CN114196123A (en) * | 2021-12-08 | 2022-03-18 | 南京理工大学 | Anti-migration ethylene propylene diene monomer rubber heat insulation layer |
| CN114605761B (en) * | 2022-04-02 | 2023-06-27 | 宁国市瑞普密封件有限公司 | Low-pressure acrylate-changing rubber product material and preparation method thereof |
| CN115534368B (en) * | 2022-09-21 | 2024-04-05 | 湖北航天化学技术研究所 | Preparation method of graphene-based migration-preventing layer |
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| CN103865130A (en) * | 2014-03-31 | 2014-06-18 | 青岛四方车辆研究所有限公司 | High-damping rubber support base and manufacturing method thereof |
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