CN104877175B - A kind of supermolecule damping agent and its preparation method and application - Google Patents
A kind of supermolecule damping agent and its preparation method and application Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
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- 239000000463 material Substances 0.000 claims abstract description 31
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- 239000001257 hydrogen Substances 0.000 claims abstract description 26
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 23
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 20
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- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 claims description 9
- 229920000877 Melamine resin Polymers 0.000 claims description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 241000549556 Nanos Species 0.000 claims description 7
- AKXUUJCMWZFYMV-UHFFFAOYSA-M tetrakis(hydroxymethyl)phosphanium;chloride Chemical compound [Cl-].OC[P+](CO)(CO)CO AKXUUJCMWZFYMV-UHFFFAOYSA-M 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
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- 238000007098 aminolysis reaction Methods 0.000 claims 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 235000021355 Stearic acid Nutrition 0.000 description 6
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 6
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 6
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- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 3
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
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- JBIROUFYLSSYDX-UHFFFAOYSA-M benzododecinium chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 JBIROUFYLSSYDX-UHFFFAOYSA-M 0.000 description 2
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- CUXQLKLUPGTTKL-UHFFFAOYSA-M microcosmic salt Chemical compound [NH4+].[Na+].OP([O-])([O-])=O CUXQLKLUPGTTKL-UHFFFAOYSA-M 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of supermolecule damping agent and its preparation method and application.Described supermolecule damping agent is to be obtained by multiple hydrogen bonding supermolecule polymer with inorganic nano montmorillonite by cation exchange, intercalation, self assembly.Supermolecule damping agent of the present invention realizes the synergistic function of montmorillonite and multiple hydrogen bonding supermolecule polymer, not only with excellent mechanical property and heat resistance, and damping capacity is significantly improved；After tested, damping capacity, anti-wear performance and the mechanical property of the damping rubber material prepared using supermolecule damping agent of the present invention are improved significantly.It is reproducible in addition, damping agent of the present invention also has preparation technology simple, it is easy to accomplish the advantages of scale.
Description
Technical field
It is to be related to a kind of supermolecule damping agent specifically the present invention relates to a kind of damping agent and its preparation method and application
And its preparation method and application, belong to damping material technical field.
Background technology
Damping material is the material that solid mechanical vibrational energy is changed into heat energy and dissipated, and is mainly used in vibration and noise control
System.As people increasingly pay attention to the pollution caused by noise and harm, the vibration damping, anti-acoustic capability to damping material are consequently also
Propose requirements at the higher level.
Supermolecule polymer (Supermolecule polymer) is monomeric unit with reversible and height-oriented non-covalent
Interact the polymer that is combined into, according to the difference of combination, supermolecule polymer can be divided into coordination polymer, π-
Pi accumulation polymer and the class of Hydrogenbond polymer three.Due to the directionality and intensity of non-covalent bond, this kind of polymer is shown perhaps
More interesting function, for example：Stimulating responsive and nanostructured self assembly characteristic.In recent years, supermolecule polymer has turned into poly-
The important research direction of compound scientific domain, supermolecule polymer not only has the performance of traditional polymer, and due to oversubscription
The dynamic reversible characteristic of subsystem, the performance of this kind of polymer can be regulated and controled by environmental stimuli, and it is specific to assign material
Function.Multiple hydrogen bonding combination supermolecule polymer is improving polymer performance, is forming complicated molecule construction, self-assembled nanometer
Important function is shown in terms of structure, it has also become the wide concerned supermolecule polymer of a class, but so far there are no such oversubscription
Application report of the sub- polymer in damping material.
The content of the invention
In view of the above-mentioned problems existing in the prior art, it is an object of the invention to provide a kind of supermolecule damping agent and its preparation
Methods and applications, realize application of the supermolecule polymer in damping material.
For achieving the above object, the technical solution adopted by the present invention is as follows：
A kind of supermolecule damping agent, is to be handed over by multiple hydrogen bonding supermolecule polymer and inorganic nano montmorillonite by cation
Change, intercalation, self assembly are obtained.
As a kind of preferred scheme, described multiple hydrogen bonding supermolecule polymer is by melamine and polyimides quaternary phosphonium
Salt is prepared by triple Hydrogenbonds.
As further preferred scheme, described multiple hydrogen bonding supermolecule polymer is by melamine and polyimides season
Microcosmic salt in halogenated hydrocarbon solvent (for example：Dichloromethane, chloroform) in, obtain in stirring reaction at 40~60 DEG C.
Wherein：The mol ratio of polyimides quaternary alkylphosphonium salt and melamine is preferably 1:(1~1.2).
As further preferred scheme, described polyimides quaternary alkylphosphonium salt is first to carry out amine with ammonia by trimellitic anhydride
Solution reaction, then carries out esterification with THPC and is made.
As still more preferably scheme, the preparation of described polyimides quaternary alkylphosphonium salt comprises the following steps：
Trimellitic anhydride is added into organic solvent (for example：Thionyl chloride) in, in the case where being passed through ammonia, in 50~70 DEG C of stirrings
Reaction 4~6 hours；Then THPC is added, is reacted 4~6 hours at 120~140 DEG C.
Wherein：The mol ratio of trimellitic anhydride and ammonia is preferably 1:(1~1.5)；Trimellitic anhydride and tetra methylol chlorine
The mol ratio for changing phosphorus is 1:(3.5~4).
The preparation method of supermolecule damping agent of the present invention, comprises the following steps：By inorganic nano montmorillonite with it is many
Deuterium bond supermolecule polymer is in ethanol water, in stirring reaction 4~6 hours at 60~70 DEG C.
As a kind of preferred scheme, the montmorillonite of 100g inorganic nanos adds the polymerization of 0.08~0.1mol multiple hydrogen bondings supermolecule
Thing.
The volume fraction of described ethanol water is 10%~90%, preferably 30%~70%.
A kind of damping rubber material for applying supermolecule damping agent of the present invention to prepare, it is characterised in that：In 100 matter
In the rubber matrix for measuring part, added with 5~20 mass parts supermolecule damping agent of the present invention.
As a kind of preferred scheme, the composition of described damping rubber material and match as follows：
Described rubber matrix is preferably at least one of neoprene, ethylene propylene diene rubber and nitrile rubber.
Described vulcanizing agent is preferably sulphur.
A kind of method for preparing described damping rubber material, is to add each constituent of proportional quantity in mill,
Kneaded at 40~60 DEG C.
The montmorillonite that the present invention is used can use commercialized inorganic nano montmorillonite product, such as Zhejiang Feng Hong clays
The inorganic nano montmorillonite product of the SMP trades mark of Co., Ltd's production.
Compared with prior art, the present invention has following conspicuousness progress：
Because supermolecule damping agent of the present invention is by making multiple hydrogen bonding supermolecule polymer be covered with inorganic nano
De- soil is obtained by cation exchange, intercalation, self assembly, can be formed and cooperateed between montmorillonite and multiple hydrogen bonding supermolecule polymer
Synergistic effect, can not only improve the mechanical property and heat resistance of material, and because of the presence of a large amount of hydrogen bonds, can make the resistance of material
Damping properties are significantly improved；After tested, the damping rubber material prepared using supermolecule damping agent of the present invention has
Excellent damping capacity, anti-wear performance and mechanical property, with wide application prospect.In addition, damping agent of the present invention is also
It is simple with preparation technology, it is reproducible, it is easy to accomplish the advantages of scale.
Embodiment
Technical solution of the present invention is described in further detail and completely with reference to embodiment and comparative example.
The particle size of supermolecule damping agent is observed using transmission electron microscope method.
Using《Nano composite polymer/laminated silicate material theory and practice》(QiZongNeng, Shang Wenyu writes chemical work
Industry publishing house, 2002) thermogravimetry, test supermolecule damping agent thermal weight loss central temperature.
The DMA-242 types dynamic mechanical analysis produced using German Nai Chi companies tests the damping energy of rubber.
The tensile property and wear hardness of rubber are tested using GB 528-83 and GB/T1689-1998.
Embodiment 1
First, the preparation of polyimides quaternary alkylphosphonium salt：7.5g trimellitic anhydrides (CAS#552-30-7) are added to equipped with 50mL
In the sealed there-necked flask of thionyl chloride, 0.75L ammonias are then passed through into there-necked flask, then insulated and stirred is reacted at 50 DEG C
5h, 6.5mL THPCs (CAS#124-64-1) are then added into there-necked flask, 120 DEG C, then insulated and stirred is warming up to
5h is reacted, terminates reaction, rotary evaporation removes solvent, and obtained yellowish color substance is polyimides quaternary alkylphosphonium salt.
2nd, the preparation of multiple hydrogen bonding supermolecule polymer：By 4g melamines (CAS#108-78-1) and obtained polyamides
Imines quaternary alkylphosphonium salt is added in 50mL chloroforms, and stirring makes to be well mixed, then the insulation reaction 3h at 50 DEG C；Remove molten
Agent, crystallisation by cooling, and rinse product 3 times with acetone solvent, dry, that is, obtain described multiple hydrogen bonding supermolecule polymer.
3rd, the preparation of supermolecule damping agent：By the montmorillonite of 30g inorganic nanos and obtained multiple hydrogen bonding supermolecule polymer
It is added in 100mL ethanol waters, stirring makes to be well mixed, then the insulation reaction 5h at 65 DEG C；Terminate reaction, suction filtration is received
Collect solid, dry, that is, obtain described supermolecule damping agent.
It is shown in Table 1 on the average grain diameter of gained supermolecule damping agent and the test data of thermal weight loss temperature.
Application examples 1
By 100g chlorinated scolines, 3g sulphur, 1.5g captaxs, 0.3g Vulcanization accelerator TMTDs, 0.8g stearic acid, 4.8g
Zinc oxide, 1g antioxidant Ds and supermolecule damping agent made from 10g this example are added in mill, are kneaded, produced at 40 DEG C
To damping rubber material of the present invention.
Performance test data on prepared damping rubber material is shown in Table 2.
Comparative example 1
By 100g chlorinated scolines, 3g sulphur, 1.5g captaxs, 0.3g Vulcanization accelerator TMTDs, 0.8g stearic acid, 4.8g
Zinc oxide, 1g antioxidant Ds are added in mill, are kneaded at 40 DEG C, obtain contrasting damping rubber material.
Performance test data on prepared contrast damping rubber material is also shown in Table 2.
Embodiment 2
First, the preparation of polyimides quaternary alkylphosphonium salt：9g trimellitic anhydrides (CAS#552-30-7) are added to equipped with 50mL chlorine
In the sealed there-necked flask for changing sulfoxide, 0.9L ammonias are then passed through into there-necked flask, then insulated and stirred reacts 5h at 60 DEG C,
Then 7.5mL THPCs (CAS#124-64-1) are added into there-necked flask, 130 DEG C are warming up to, then insulated and stirred is anti-
5h is answered, terminates reaction, rotary evaporation removes solvent, and obtained yellowish color substance is polyimides quaternary alkylphosphonium salt.
2nd, the preparation of multiple hydrogen bonding supermolecule polymer：By 6g melamines (CAS#108-78-1) and obtained polyamides
Imines quaternary alkylphosphonium salt is added in 50mL chloroforms, and stirring makes to be well mixed, then the insulation reaction 3h at 50 DEG C；Remove molten
Agent, crystallisation by cooling, and rinse product 3 times with acetone solvent, dry, that is, obtain described multiple hydrogen bonding supermolecule polymer.
3rd, the preparation of supermolecule damping agent：By the montmorillonite of 40g inorganic nanos and obtained multiple hydrogen bonding supermolecule polymer
It is added in 100mL ethanol waters, stirring makes to be well mixed, then the insulation reaction 5h at 65 DEG C；Terminate reaction, suction filtration is received
Collect solid, dry, that is, obtain described supermolecule damping agent.
It is shown in Table 1 on the average grain diameter of gained supermolecule damping agent and the test data of thermal weight loss temperature.
Application examples 2
By 100g chlorinated scolines, 3g sulphur, 1.5g captaxs, 0.3g Vulcanization accelerator TMTDs, 0.8g stearic acid, 4.8g
Zinc oxide, 1g antioxidant Ds and supermolecule damping agent made from 15g this example are added in mill, are kneaded, produced at 40 DEG C
To damping rubber material of the present invention.
Performance test data on prepared damping rubber material is shown in Table 2.
Comparative example 2
60mL quaternary ammonium salts (the alkyl quaternary ammonium salts such as cetyl trimethylammonium bromide, dodecyl dimethyl benzyl ammonium chloride
Can) 2h is reacted at 60~70 DEG C with the montmorillonite of 40g inorganic nanos, modified organo montmorillonite is made.
By 100g chlorinated scolines, 3g sulphur, 1.5g captaxs, 0.3g Vulcanization accelerator TMTDs, 0.8g stearic acid, 4.8g
Zinc oxide, 1g antioxidant Ds and the above-mentioned modified organo montmorillonites of 15g are added in mill, are kneaded, are obtained to resistivity at 40 DEG C
Buddhist nun's elastomeric material.
Performance test data on prepared contrast damping rubber material is also shown in Table 2.
Embodiment 3
First, the preparation of polyimides quaternary alkylphosphonium salt：10g trimellitic anhydrides (CAS#552-30-7) are added to equipped with 50mL chlorine
In the sealed there-necked flask for changing sulfoxide, 1.0L ammonias are then passed through into there-necked flask, then insulated and stirred reacts 5h at 70 DEG C,
Then 9.0mL THPCs (CAS#124-64-1) are added into there-necked flask, 140 DEG C are warming up to, then insulated and stirred is anti-
5h is answered, terminates reaction, rotary evaporation removes solvent, and obtained yellowish color substance is polyimides quaternary alkylphosphonium salt.
2nd, the preparation of multiple hydrogen bonding supermolecule polymer：By 8g melamines (CAS#108-78-1) and obtained polyamides
Imines quaternary alkylphosphonium salt is added in 50mL chloroforms, and stirring makes to be well mixed, then the insulation reaction 3h at 50 DEG C；Remove molten
Agent, crystallisation by cooling, and rinse product 3 times with acetone solvent, dry, that is, obtain described multiple hydrogen bonding supermolecule polymer.
3rd, the preparation of supermolecule damping agent：By the montmorillonite of 50g inorganic nanos and obtained multiple hydrogen bonding supermolecule polymer
It is added in 100mL ethanol waters, stirring makes to be well mixed, then the insulation reaction 5h at 65 DEG C；Terminate reaction, suction filtration is received
Collect solid, dry, that is, obtain described supermolecule damping agent.
It is shown in Table 1 on the average grain diameter of gained supermolecule damping agent and the test data of thermal weight loss temperature.
Application examples 3
By 100g chlorinated scolines, 3g sulphur, 1.5g captaxs, 0.3g Vulcanization accelerator TMTDs, 0.8g stearic acid, 4.8g
Zinc oxide, 1g antioxidant Ds and supermolecule damping agent made from 20g this example are added in mill, are kneaded, produced at 40 DEG C
To damping rubber material of the present invention.
Performance test data on prepared damping rubber material is shown in Table 2.
Comparative example 3
60mL quaternary ammonium salts (the alkyl quaternary ammonium salts such as cetyl trimethylammonium bromide, dodecyl dimethyl benzyl ammonium chloride
Can) 3h is reacted at 60~70 DEG C with the montmorillonite of 60g inorganic nanos, modified organo montmorillonite is made.
By 100g chlorinated scolines, 3g sulphur, 1.5g captaxs, 0.3g Vulcanization accelerator TMTDs, 0.8g stearic acid, 4.8g
Zinc oxide, 1g antioxidant Ds and the above-mentioned modified organo montmorillonites of 20g are added in mill, are kneaded, are obtained to resistivity at 40 DEG C
Buddhist nun's elastomeric material.
Performance test data on prepared contrast damping rubber material is also shown in Table 2.
The average grain diameter and thermal weight loss temperature of the supermolecule damping agent of table 1
| Sample | Average grain diameter/nm | Thermal weight loss central temperature/DEG C |
| Embodiment 1 | 30~40 | 250~300 |
| Embodiment 2 | 40~55 | 300~350 |
| Embodiment 3 | 55~70 | 350~400 |
From table 1：The supermolecule damping agent of the present invention is nano material, with very high heat endurance.
The performance test data of the damping rubber material of table 2
| Sample | tanδ | Tensile strength/MPa | Elongation at break/% | Wear volume/cm3 |
| Application examples 1 | 1.2 | 7.0 | 800 | 0.12 |
| Comparative example 1 | 0.8 | 5.8 | 650 | 0.16 |
| Application examples 2 | 1.4 | 7.4 | 840 | 0.09 |
| Comparative example 2 | 1.0 | 6.0 | 700 | 0.14 |
| Application examples 3 | 1.6 | 7.8 | 900 | 0.07 |
| Comparative example 3 | 1.2 | 6.2 | 750 | 0.12 |
From table 2：The damping rubber material that the present invention is provided has excellent damping capacity, mechanical property and wearability
Energy.
In summary：By the present invention in that multiple hydrogen bonding supermolecule polymer is handed over inorganic nano montmorillonite by cation
Change, intercalation, self assembly prepare supermolecule damping agent, the synergy with montmorillonite Yu multiple hydrogen bonding supermolecule polymer,
Not only there is good mechanical property and heat resistance, and with excellent damping capacity.By the application examples in table 2 and contrast
The test result of example is can be found that：The elastomeric material of the supermolecule damping agent of the addition present invention is not than adding montmorillonite and only adding
Enter the elastomeric material of modified montmorillonite (modified montmorillonoid do not carried out with supramolecular materials further combined with), its each side
Performance is all significantly increased；With the increase of supermolecule damping agent usage amount of the present invention, the damping and amortization of obtained elastomeric material and
Mechanical property is improved therewith.
Finally need described herein be：Neoprene in application examples of the present invention could alternatively be ethylene propylene diene rubber or
Nitrile rubber.In above-described embodiment, the volume fraction of described ethanol water can be 10%~90%, preferably 40%~
70%.
In a word, above example is served only for being described in more detail technical scheme, it is impossible to be interpreted as
Limiting the scope of the invention, those skilled in the art according to the above of the present invention make some are nonessential
Modifications and adaptations belong to protection scope of the present invention.
Claims (9)
1. a kind of supermolecule damping agent, it is characterised in that：It is to be passed through by multiple hydrogen bonding supermolecule polymer and inorganic nano montmorillonite
Cation exchange, intercalation, self assembly is crossed to obtain；Described multiple hydrogen bonding supermolecule polymer is by melamine and polyimides
Quaternary alkylphosphonium salt is prepared by triple Hydrogenbonds.
2. supermolecule damping agent according to claim 1, it is characterised in that：Described multiple hydrogen bonding supermolecule polymer is
Obtained by melamine with polyimides quaternary alkylphosphonium salt in halogenated hydrocarbon solvent, in stirring reaction at 40~60 DEG C.
3. supermolecule damping agent according to claim 1 or 2, it is characterised in that：Described polyimides quaternary alkylphosphonium salt is logical
Cross trimellitic anhydride and first carry out aminolysis reaction with ammonia, then carrying out esterification with THPC is made.
4. supermolecule damping agent according to claim 3, it is characterised in that the preparation bag of described polyimides quaternary alkylphosphonium salt
Include following steps：Trimellitic anhydride is added in organic solvent, in the case where being passed through ammonia, small in 50~70 DEG C of stirring reactions 4~6
When；Then THPC is added, is reacted 4~6 hours at 120~140 DEG C.
5. the preparation method of the supermolecule damping agent described in a kind of claim 1, it is characterised in that comprise the following steps：By nothing
Machine nano imvite with multiple hydrogen bonding supermolecule polymer in ethanol water, it is small in stirring reaction 4~6 at 60~70 DEG C
When.
6. preparation method according to claim 5, it is characterised in that：100g inorganic nanos montmorillonite addition 0.08~
0.1mol multiple hydrogen bonding supermolecule polymers.
7. damping rubber material prepared by the supermolecule damping agent described in a kind of application claim 1, it is characterised in that：100
In the rubber matrix of mass parts, added with the supermolecule damping agent described in 5~20 mass parts.
8. damping rubber material according to claim 7, it is characterised in that with following composition and proportioning：
9. the damping rubber material according to claim 7 or 8, it is characterised in that：Described rubber matrix be neoprene,
At least one of ethylene propylene diene rubber and nitrile rubber.
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| CN1908036A (en) * | 2006-07-26 | 2007-02-07 | 华南理工大学 | Preparation method of hydrogen bond composite inorganic-organic hybridization network modified polymer |
| CN103834197A (en) * | 2014-03-18 | 2014-06-04 | 上海工程技术大学 | Preparation method of organic montmorillonite modified by supermolecular liquid crystal polymer |
| CN104292506A (en) * | 2014-10-03 | 2015-01-21 | 上海工程技术大学 | Hyperbranched damping agent as well as preparation method and application thereof |
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| CN103834197A (en) * | 2014-03-18 | 2014-06-04 | 上海工程技术大学 | Preparation method of organic montmorillonite modified by supermolecular liquid crystal polymer |
| CN104292506A (en) * | 2014-10-03 | 2015-01-21 | 上海工程技术大学 | Hyperbranched damping agent as well as preparation method and application thereof |
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