CN107698916A - Wide temperature range ACM base graphene oxide damping material and preparation method thereof - Google Patents
Wide temperature range ACM base graphene oxide damping material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/29—Compounds containing one or more carbon-to-nitrogen double bonds
- C08K5/31—Guanidine; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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Abstract
The invention discloses a kind of wide temperature range ACM base graphene oxide damping material and preparation method thereof.Its step is：By adjusting oxidizer, certain size is prepared, surface carries the graphene oxide dispersion of a large amount of polar groups；ACM is mixed with the various compounding ingredients such as hindered phenol small molecule, vulcanizing agent using mechanical blending method, then mixed using solution blended process with graphene oxide, is dried, vulcanization, you can obtain the ACM base damping rubbers of the wide temperature range containing graphene oxide of the present invention.The present invention is carried using surface forms strong hydrogen bond between graphene oxide, hindered phenol small molecule and the ACM of a large amount of polar groups, while utilizes the barrier property of graphene oxide, substantially increases the effective damping temperature range of ACM base graphene oxide damping materials（tanδ≥0.3）And its damping capacity after aging.
Description
Technical field
The invention belongs to technical field prepared by damping material, and in particular to a kind of wide temperature range ACM（ACM）
Base graphene oxide damping material and preparation method thereof.
Background technology
With the development of contemporary industry technology, every field gradually realizes the mechanization and automation of production.Although this
Brought great convenience to our production and life, but its adjoint vibration and noise also to our health and
Mental health brings great hidden danger, while vibration can also have a strong impact on the service life for influenceing plant equipment, improves equipment
Maintenance cost.So damping noise reduction becomes current urgent problem.It is the master for solving the problem using damping material
Want one of means.Visco-elastic damping material as a kind of material that vibrational energy and acoustic energy can be largely changed into thermal energy consumption and dissipated,
It is a kind of excellent damping damping material.
At present, in visco-elastic damping material research field, it is primarily present following problem：（1）Visco-elastic damping material
Good damping capacity is mainly near glass transition temperature, but relatively low glass transition temperature（Major part is 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
Energy（Fissipation factor tanδ≥0.3）And wide effective damping temperature range（tanδ>=0.3 temperature range）Two conditions；（3）Resistance
Buddhist nun's process is the process that kinetic energy is converted into heat energy, therefore in actual use, rubber internal heat steeply rises, on the one hand
Easily cause the migration of small molecule damping agent to be lost in, lose damping, on the other hand cause the aging of rubber molecular chain.Cause
How this, solve the above problems, be to prepare one of study hotspot of damping rubber simultaneously.
The content of the invention
It is an object of the invention to provide one kind to have the wide temperature range of high-damping, still has the resistance of preferable damping capacity after aging
Damping material and preparation method thereof.
Realize that the technical solution of the present invention is as follows：
Described wide temperature range ACM base graphene oxide damping material, in terms of mass parts, includes ACM
100 parts, 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 age resistor, 2~4 parts of processing aid, 1~4 part of vulcanizing agent.
Wherein, described hindered phenol small molecule is any one in AO-60 and AO-80 or two kinds.
Described vulcanization accelerator is 1,3- diphenylguanidine（D）With 1,3- bis--o- tolyl guanidine（DOTG）In any one
Or two kinds.
Described age resistor is N- isopropyl-N'- diphenyl-para-phenylene diamines（4010NA）And N, N'- diphenyl-para-phenylene diamine
（DPPD）In any one or two kinds.
Described processing aid is any one or a few in RL210, WS280 and WB222.
Described vulcanizing agent is Sulfur.
The preparation method of the above-mentioned acrylate-based graphene oxide damping material of wide temperature range, comprises the following steps：
Step 1, large scale, high oxidation degree graphene oxide are prepared using improved Hummers methods, 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 (DMSO) mixed solution, decompression
Distillation is until obtain the dimethyl sulphoxide solution of graphene oxide；
Step 3, by ACM and hindered phenol small molecule, stearic acid, vulcanization accelerator, age resistor, processing aid and sulphur
Agent is kneaded, then thin pass-out piece；Cooling, is ground into fine particle, is then dissolved in dimethyl sulphoxide solution；
Step 4, solution blending step 2 and step 3 obtained, after drying, wide temperature range ACM bases graphene oxide resistance is made in vulcanization
Damping material.
Further, in step 2, water and dimethyl sulfoxide (DMSO) mixed solution reclaimed water and the volume ratio of dimethyl sulfoxide (DMSO) are 1:1,
4~6mg/mL of concentration of the dimethyl sulphoxide solution of graphene oxide.
Compared with prior art, its remarkable advantage is the present invention：
（1）Ratio of the invention by adjusting potassium permanganate and graphite, obtain large scale, individual layer and surface and carry a large amount of oxygen-containing groups
The graphene oxide of group, using solution blending, graphene oxide and ACM can be mixed uniformly；Utilize large scale graphene oxide
Constraint to the strand of rubber, improve the glass transition temperature of elastomeric material.
（2）The present invention utilizes specific accelerator 1,3- diphenylguanidine（D）And/or 1,3- bis--o- tolyl guanidine（DOTG）With
Interaction between graphene oxide, hindered phenol small molecule, formed between graphene oxide, hindered phenol and its ACM strong
Hydrogen bond action, using the iris 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）The specific age resistor N- isopropyls-N'- diphenyl-para-phenylene diamines of the present invention（4010NA）And/or N, N'- hexichol
Base p-phenylenediamine（DPPD）The weak bond of varying strength closes between graphene oxide and small molecule damping agent, i.e., at different temperatures
The weak bond for having varying strength closes so that and within the scope of wider temperature, there are enough weak bonds to close and fracture occurs with being bonded again, from
And widen effective damping temperature range.
（4）When filling 0.5 part of graphene oxide and during 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.
Brief description of the drawings
Fig. 1 is the preparation flow schematic diagram of the wide temperature range ACM bases graphene oxide damping material prepared by embodiment 1.
Fig. 2 is the AFM figures of the large scale graphene oxide prepared by embodiment 1（a）And its corresponding height map（b）.
Fig. 3 is the full spectrograms of XPS of the large scale graphene oxide prepared by embodiment 1（a）And its C1s XPS spectrum figures（b）.
Fig. 4 is wide temperature range ACM base graphene oxide damping materials prepared by embodiment 1 in 100 °C of lower agings 48 hours
Front and rear DMA comparison diagrams.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
The ACM used in following examples（ACM rubber）To be commercially available, damping of its trade mark to damping material
Performance has no significant effect.
The method of the invention for mainly using mechanical blending+solution blending, remains big chi of the graphene oxide in rubber
Very little pattern, by controlling size, individual layer and the degree of oxidation of graphene oxide, on the one hand utilize large-sized graphene oxide pair
Effective constraint of rubber molecular chain, improve the glass transition temperature of elastomeric material；On the other hand surface of graphene oxide is utilized
Active function groups, between small molecule damping agent and accelerator forming the different weak bond of intensity closes, and improves the damping and amortization of rubber
Can, meanwhile, further closed using the weak bond of varying strength between age resistor and graphene oxide and small molecule damping agent, i.e., not
The weak bond for having varying strength under synthermal closes so that within the scope of wider temperature, have enough weak bond close occur fracture with
It is bonded again, so as to widen effective damping temperature range；Moreover, large-sized graphene oxide, which can manage it, forms good thermal conducting path
With barrier path, by while caused heat is dissipated to the external world in damping process, moving for damping agent small molecule is effectively prevented
Move loss.
Embodiment 1
Step 1, the 230 mL concentrated sulfuric acids are measured in four-hole boiling flask, ice bath, are down to 0 °C or so.Sequentially add 10 g graphite, 5 g
Sodium nitrate, the min of agitating solution 15.Then 30 g potassium permanganate are slowly added in three times in 1 h, keeping temperature is less than 20 °
C.35 °C are warming up to after well mixed, is kept stirring for 2 h.460 mL deionized waters are slowly added to afterwards, in this process,
Keep solution temperature to be less than 100 °C, keep 15 min, liquid is transferred in beaker, add 750 mL deionized waters and 250
ML 5% hydrogenperoxide steam generator.Then arrive graphene oxide through ultrasound, dialysis, drying and processing, and to graphene oxide progress
Characterize, AFM figures and its corresponding height map are as shown in Fig. 2 XPS figures are as shown in Figure 3；
Step 2, the large-sized graphene oxides of 0.5 g step 1 obtained, put into water and dimethyl sulfoxide (DMSO) mixed solution,
Ultrasound, graphene oxide is dispersed in water mixed solution, be evaporated under reduced pressure and obtain the graphene oxide that concentration is 5mg/mL
Dimethyl sulphoxide solution；
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 parts anti-
Old agent 4010NA, 2 parts of processing aid RL210, the formula of 1 part of Sulfur are kneaded, then thin pass-out piece.Cooling, is ground into tiny
Grain, is then dissolved in dimethyl sulphoxide solution；
Step 4, the solution blending that step 2 and step 3 obtain, after drying, its sulfurizing time is determined with vulcameter, according to sulfuric
Change time vulcanization and wide temperature range ACM bases graphene oxide damping material is made.
DMA contrast of the wide temperature range ACM base graphene oxide damping materials prepared before and after 100 °C of lower agings 48 hours
Figure is as shown in Figure 4.As a result at -8.1 DEG C~38.4 DEG C, temperature range width reaches the effective damping temperature range for the damping material for finding to obtain
46.5 DEG C, the damping temperature domain of material can also reach 44.2 DEG C after aging.
Embodiment 2
The method of embodiment 1 is repeated, but in step 1, potassium permanganate dosage is 21 g；Graphene oxide dosage is in step 2
0.4 g；Mixing formula is 100 parts of ACM rubber in step 3, and 50 parts of hindered phenol small molecule AO-80,3 parts of stearic acid, 2 parts vulcanize
Diphenylguanidine, 4 parts of accelerator DOTGs, 2 parts of antioxidant 4010NAs, 3 parts of antioxidant DPPDs, 1 part of processing aid RL210,3 parts
Processing aid WS280,4 parts of Sulfurs.At -7.2 DEG C~38.0 DEG C, temperature range width reaches the effective damping temperature range of obtained damping material
To 45.2 DEG C, the damping temperature domain of material can also reach 42.4 DEG C after aging.
Embodiment 3
The method of embodiment 1 is repeated, but in step 1, potassium permanganate dosage is 15 g；Graphene oxide dosage is in step 2
0.3 g；Mixing formula is 100 parts of ACM rubber in step 3, and 30 parts of hindered phenol small molecule AO-60,2 parts of stearic acid, 2 vulcanize rush
Enter agent DOTG, 3 parts of antioxidant DPPDs, 2 parts of processing aid WB222,1 part of processing aid WS280,3 parts of Sulfurs.Obtained damping material
For the effective damping temperature range of material at -6.8 DEG C~37.8 DEG C, temperature range width reaches 44.6 DEG C, the damping temperature domain of material after aging
42.7 DEG C can be reached.
Embodiment 4
The method of embodiment 1 is repeated, but in step 1, potassium permanganate dosage is 10 g；Graphene oxide dosage is in step 2
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 of hindered phenol small molecules
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.Obtain
For the effective damping temperature range of damping material at -7.4 DEG C~37.0 DEG C, temperature range width reaches 44.2 DEG C, the damping of material after aging
Temperature range can also reach 43.0 DEG C.
Embodiment 5
The method of embodiment 1 is repeated, but in step 1, potassium permanganate dosage is 15 g；Graphene oxide dosage is in step 2
0.1 g；Mixing formula is 100 parts of ACM rubber in step 3, and 20 parts of hindered phenol small molecule AO-80,1 part of stearic acid, 4 vulcanize rush
Enter agent D, 3 parts of antioxidant DPPDs, 3 parts of processing aid WS280,4 parts of Sulfurs.The effective damping temperature range of obtained damping material-
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
The method of embodiment 1 is repeated by each component content specified, but is free from graphene oxide.As a result find, damped
The effective damping temperature range of material is at -4.2 DEG C~32.9 DEG C, and temperature range width is 37.1 DEG C, after aging under the damping temperature domain of material
Drop to 18.5 DEG C.
Comparative example 2
The method that embodiment 1 is repeated by each component content specified, but directly by graphene oxide prepared by step 1 with
ACM, AO-80, stearic acid, D, 4010NA, RL210, Sulfur carry out mixing vulcanization and damping material are prepared.As a result find, obtain
To damping material effective damping temperature range at -4.5 DEG C~33.7 DEG C, temperature range width is 38.2 DEG C, the damping of material after aging
Temperature range drops significantly to 25.5 DEG C.
Comparative example 3
The method that embodiment 1 is repeated by each component content specified, but the dosage of potassium permanganate is 40 g in step 1.Obtain
For the effective damping temperature range of damping material at -9.8 DEG C~30.8 DEG C, temperature range width is 40.6 DEG C, the damping temp of material after aging
Domain drops significantly to 26.7 DEG C.
Comparative example 4
The method of embodiment 1 is repeated by each component content specified, but is free from hindered phenol small molecule.Obtain damping material has
Damping temperature domain is imitated at -5.2 DEG C~33.4 DEG C, temperature range width is 38.6 DEG C, and the damping temperature domain of material drops significantly to after aging
22.5℃。
Comparative example 5
The method that embodiment 1 is repeated by each component content specified, but age resistor is 2,2,4- trimethyl -1,2- dihydros
Change quinoline 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
The method that embodiment 1 is repeated by each component content specified, but accelerator is the N- tert-butyl groups -2-[4-morpholinodithio time sulphonyl
Amine（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, material after aging
The damping temperature domain of material drops significantly to 27.3 DEG C.
Comparative example 7
The method that embodiment 1 is repeated by each component content specified, but graphene oxide dosage is 1 g.Obtain damping material
Effective damping temperature range at -10.6 DEG C~29.6 DEG C, temperature range width is 40.2 DEG C, under the damping temperature domain of material is notable after aging
Drop to 30.5 DEG C.
Claims (9)
1. wide temperature range ACM base graphene oxide damping material, it is characterised in that in terms of mass parts, include acrylic acid
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 age resistor, 2~4 parts of processing aid, 1~4 part of vulcanizing agent.
2. damping material as claimed in claim 1, it is characterised in that described hindered phenol small molecule is in AO-60 and AO-80
Any one or two kinds.
3. damping material as claimed in claim 1, it is characterised in that described vulcanization accelerator is 1,3- diphenylguanidine and 1,3-
Any one in two-o- tolyl guanidine or two kinds.
4. damping material as claimed in claim 1, it is characterised in that described age resistor is N- isopropyl-N'- phenyl to benzene
Any one in diamines and N, N'- diphenyl-para-phenylene diamine or two kinds.
5. damping material as claimed in claim 1, it is characterised in that described processing aid is RL210, WS280 and WB222
In any one or a few.
6. damping material as claimed in claim 1, it is characterised in that described vulcanizing agent is Sulfur.
7. the preparation method of the acrylate-based graphene oxide damping material of wide temperature range as described in claim 1-6 is any, its
It is characterised by, comprises the following steps：
Step 1, large scale, high oxidation degree graphene oxide are prepared using improved Hummers methods, 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 evaporated under reduced pressure in water and dimethyl sulfoxide (DMSO) mixed solution
Until obtaining the dimethyl sulphoxide solution of graphene oxide；
Step 3, by ACM and hindered phenol small molecule, stearic acid, vulcanization accelerator, age resistor, processing aid and sulphur
Agent is kneaded, then thin pass-out piece；Cooling, is ground into fine particle, is then dissolved in dimethyl sulphoxide solution；
Step 4, solution blending step 2 and step 3 obtained, after drying, wide temperature range ACM bases graphene oxide resistance is made in vulcanization
Damping material.
8. method as claimed in claim 7, it is characterised in that in step 2, water and dimethyl sulfoxide (DMSO) mixed solution reclaimed water and two
The volume ratio of methyl sulfoxide is 1:1.
9. method as claimed in claim 7, it is characterised in that in step 2, the dimethyl sulphoxide solution of graphene oxide it is dense
Spend 4~6mg/mL.
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Cited By (7)
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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 |
| CN110256795A (en) * | 2019-05-17 | 2019-09-20 | 浙江工业大学 | Novel high fire protecting performance damping material of olefinic carbon and the preparation method and application thereof |
| CN112210216A (en) * | 2020-08-31 | 2021-01-12 | 四川中物材料股份有限公司 | High-damping phenyl silicone rubber and preparation method and application thereof |
| CN112300525A (en) * | 2020-10-27 | 2021-02-02 | 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 |
| CN114605761A (en) * | 2022-04-02 | 2022-06-10 | 宁国市瑞普密封件有限公司 | Low-pressure-change acrylate rubber product material and preparation method thereof |
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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 |
| CN110256795A (en) * | 2019-05-17 | 2019-09-20 | 浙江工业大学 | Novel high fire protecting performance damping material of olefinic carbon and the preparation method and application thereof |
| 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 |
| CN112210216A (en) * | 2020-08-31 | 2021-01-12 | 四川中物材料股份有限公司 | High-damping phenyl silicone rubber and 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 |
| CN112300525A (en) * | 2020-10-27 | 2021-02-02 | 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 |
| 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 |
| CN114605761A (en) * | 2022-04-02 | 2022-06-10 | 宁国市瑞普密封件有限公司 | Low-pressure-change acrylate rubber product material and preparation method thereof |
| CN115534368A (en) * | 2022-09-21 | 2022-12-30 | 湖北航天化学技术研究所 | Preparation method of graphene-based anti-migration layer |
| 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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