CN107418110A - A kind of novel vehicle graphene environmental-protection damp material and preparation method thereof - Google Patents

A kind of novel vehicle graphene environmental-protection damp material and preparation method thereof Download PDF

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CN107418110A
CN107418110A CN201710804343.7A CN201710804343A CN107418110A CN 107418110 A CN107418110 A CN 107418110A CN 201710804343 A CN201710804343 A CN 201710804343A CN 107418110 A CN107418110 A CN 107418110A
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rare earth
earth oxide
tiny balloon
novel vehicle
preparation
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CN107418110B (en
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甘国民
陈慧婷
陶宇
何孔儒
魏玉花
范晨阳
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Changzhou University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16—Fibres; Fibrils

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Vibration Prevention Devices (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention belongs to aqueous damping Material Field, more particularly to a kind of novel vehicle graphene environmental-protection damp material and preparation method thereof.Water-and acrylate, aqueous polyurethane, polysiloxanes, doughnut, the rare earth oxide tiny balloon handled by LBL self-assembly, grapheme foam, bentonite are well mixed, gained damping material has the dual sound absorbing mechanism of cavity sound absorption structure and viscoelastic damping characteristic, realize and eliminate the noise in terms of automobile-used damping material, traditional asphalt damping sheet is substituted, is had the advantages that environmentally friendly.

Description

A kind of novel vehicle graphene environmental-protection damp material and preparation method thereof
Technical field
The invention belongs to aqueous damping Material Field, more particularly to a kind of novel vehicle graphene environmental-protection damp material and its Preparation method.
Background technology
One of the problem of NVH problems of vehicle are the major vehicle manufacturing enterprise of international automobile industry and parts enterprises concern, Wherein NVH is the english abbreviation of noise, vibration and sound vibration roughness (Noise, Vibration, Harshness).There is statistics to provide Material display, the failure problems that vehicle there are about 1/3 are that have relation with the NVH problems of vehicle, and there are nearly 20% research and development in each major company Cost consumption is on the NVH for solving the problems, such as vehicle.
With the continuous improvement of people's environmental consciousness and the successive appearance of various countries' environmental regulation, green car has become The inexorable trend of future automobile development, thus automobile is met the requirement of environmental protection, it just refer to automobile vendors Agenda.And the main flow that environment-friendly type damping new material develops as future automobile damping material, it will play the part of wherein very Important role, it can predict in the near future, the composite of higher performance will be applied more broadly in automobile and iron In the locomotive field of road.In recent years, as field of traffic developing steps are accelerated, the growth of car, high ferro, subway quantity drives green wood Expect Industry Quick Development, environment-friendly type damping new material market is steadily increasing, the gradual recovery of global economy in addition, damps composite wood Material will continue to rise steadily on car and railway locomotive using quickening, the demand of damping material.
The content of the invention
The invention provides a kind of novel vehicle graphene environmental-protection damp material, main characteristic using damping material and The rational design of damping structure, reach the purpose of vibration and noise reducing, include according to the number of parts by weight：
Wherein, water-and acrylate has a preferable resistance to elevated temperatures, ageing-resistant performance, it is common as VN954, VN937, VN960、VN65、VN68、VN68S、VN710、VN605、VN610、VN650、VN825；
It is water-based poly- that aqueous polyurethane mainly includes polyether type aqueous polyurethane, polyester-type aqueous polyurethane and polyolefin-type Urethane, there is the advantages that performance such as high intensity, wear-resistant, safe and non-toxic, free from environmental pollution, such as AMS-2066,44V20, BC- 6555th, SP-90, BY-6555, PU-2890, QJ-6555, HK718, PU-3777A, IMK-800, PU-6011 etc.；
And waterborne acrylic paint can form a kind of Semi-IPN polymer network structure with aqueous polyurethane, have Mutual tolerance, interface IPN, two-way continuous and collaboration damping effect are forced,
Polysiloxanes is the organic polymer synthetic material containing elemental silicon in molecular structure, and its special molecular structure makes Polysiloxanes intermolecular interaction it is smaller and it is intermolecular higher submissive state is presented, have good hydrophily, lower temperature resistance, Lubricity and good physiological inertia, specific such as amino-polyether polysiloxanes, saccharide-modified polyetherpolysilicone, polyurethane- Polyetherpolysilicone block copolysiloxane, benzophenone polyetherpolysilicone, carboxy-modified polyetherpolysilicone etc.；
Doughnut be it is a kind of with self-supporting can, the cross section chemical fibre tubulose material with cavity vertically Material, the damping capacity and mechanical property of material can be effectively improved, it is common such as polysulfones, polyether sulfone, polyimides, poly- inclined fluorine Ethene, polypropylene, polyacrylonitrile, cellulose family, polyethers alum ketone etc.；
The preparation method of the rare earth oxide tiny balloon handled by LBL self-assembly is as follows：
(1) preparation of rare earth oxide tiny balloon
5mL~10mL polymer emulsions are added in 20mL~50mL deionized waters, after ultrasonic disperse 20min~40min, Dispersant and 5~10mol/L rare earth salt aqueous solution are added, is moved into after ultrasonic disperse in 100mL three-necked flask, is warming up to 90 After DEG C, mass concentration is added dropwise as 25~30wt% aqueous solution of urea using 0.5~1mL/min speed, drips off rear isothermal reaction 6 ~8h, filter, filter cake is washed with deionized, and is subsequently placed in 50 DEG C of thermostatic drying chamber and dries 12h, that is, obtain polymer/ Rare earth oxide complex microsphere, polymer/rare earth oxide complex microsphere is uniformly layered in crucible, crucible is put into Muffle furnace In calcine 4 hours at 500 DEG C~900 DEG C, obtain rare earth oxide tiny balloon after being cooled to room temperature (25 DEG C, similarly hereinafter),
Polymer in polymer emulsion is polystyrene, the homopolymer of polymethyl methacrylate, acrylic acid or it is common Polymers etc.,
Rare-earth salts mainly includes cerium, lanthanum, yttrium, praseodymium, gadolinium, neodymium, europium, cerium ammonium, dysprosium, scandium, erbium, terbium, an an ancient unit of weight equal to 20 or 24 *taels of silver, holmium, lutetium, the nitric acid of gallium Salt, chlorate or acetate etc.,
Dispersant is polyvinylpyrrolidone, (NH4)2SO4, stearic acid, neopelex, fatty glyceride, Fatty acid sorbitan, polysorbate etc.；
(2) LBL self-assembly is handled
The rare earth oxide tiny balloon obtained in step (1) is soaked in the solution of polyelectrolyte 1 that concentration is 1~5g/L 30~50min is steeped, 10~15min is rinsed under 0.3~0.5MPa pressure with deionized water after taking-up, is dried up；It is again that this is dilute Native hollow oxide microsphere soaks 30~50min in the solution of polyelectrolyte 2 that concentration is 1~5g/L, and deionization is used after taking-up Water rinses 10~15min under 0.3~0.5MPa pressure, drying, that is, completes double-deck deposition,
Repeat the above steps so that the number of plies that rare earth oxide tiny balloon adsorption deposition requires, to reach modification Purpose, deposition the number of plies at 10~20 layers,
Polyelectrolyte is that one kind can ionize in water, makes a kind of thing that a large amount of ionic groups are taken on macromolecular chain Matter, polyelectrolyte 1 or 2 is anion, cation or polyampholyte, while has preferable hydrophily, such as polypropylene Sour, poly- methallylsulfonic acid, PEGMA, CMCTS-g- (PAA-co-PDMDAAC), poly- (acrylic-co-acrylamide)/shell Glycan, polyvinyl pyridine, polyvinylamine etc., polyethyleneimine etc., wherein, polyelectrolyte 1 and 2 is the poly- electricity of different ions type Xie Zhi,
First, rare earth oxide tiny balloon is due to its special electronic structure (underfill of f layers), and it is in damping material Complex compound is easily formed, can effectively prevent the sub-chain motion of water-based acrylic resin, while rare earth oxide is with higher Surface energy, the macromolecule strand of low-surface-energy can be strongly adsorbed to the surface formation node of rare earth particle, hinder surrounding high The movement of strand, there is preferable damping；Meanwhile have compared to traditional rare earth oxide, hollow microsphere structure The advantages that density is low, specific surface area is high, has the magnetic energy of rare earth and the acoustic resistance characteristic of hollow material concurrently, resistance is cooperateed with grapheme foam Buddhist nun, the wave absorption to different-waveband is realized,
But microballoon is after all inorganic matter, is added in resin system and easily reunites, and causes matrix mechanical property Decline, it is therefore desirable to surface modification processing is carried out to microballoon, simply so clad by rare-earth substance and composite The molecule segment of resin is isolated from each other, and can seriously affect the interaction between rare earth oxide and polymer segment, Damping is reduced significantly,
But this patent finds the method by LBL self-assembly, although foring the considerable poly- electricity of the number of plies in microsphere surface Matter clad is solved, is repelled each other by like charges to avoid contacting with each other between microballoon, reunite, but do not have influence on rare earth oxygen Damping action of the compound to polymer segment；
Grapheme foam is a kind of loose structure film, hole size in sub-micron between several microns, special micro-structural Cause grapheme foam ultralight, there is high mechanical properties and compressibility, the formation of its special 3D macrostructure not only anti-limited step Layer occurs to reunite and stack in an assembling process, and has very big specific surface area, can effectively adsorb rare earth oxide, it is more Pore structure can effectively improve the damping capacity of material,
Bentonite has good thickening property, thixotropy, suspension stability, high-temperature stability, lubricity, film forming, resistance to Water-based and chemical stability.
Present invention also offers a kind of preparation method of above-mentioned novel vehicle graphene environmental-protection damp material：
By water-and acrylate, aqueous polyurethane, polysiloxanes, doughnut, the rare earth handled by LBL self-assembly Hollow oxide microsphere, grapheme foam, bentonite are well mixed,
Using churned mechanically hybrid mode：Mixing speed is 100~200r/min under normal temperature,
Bentonite adjusts denseness as thickener, and denseness is adjusted to 8~10.
The present invention have developed rare earth oxide/graphene aqueous, environmental protective damping material that temperature in use is wide, damping factor is high Material, there is the dual sound absorbing mechanism of cavity sound absorption structure and viscoelastic damping characteristic, realize and eliminate the noise in terms of automobile-used damping material, Traditional asphalt damping sheet is substituted, is had the advantages that environmentally friendly.
Embodiment
The rare earth oxide tiny balloon handled by LBL self-assembly used in following embodiment, by such as It is prepared by lower section method：
(1) preparation of rare earth oxide tiny balloon
8mL polymethyl methacrylates emulsion is added in 40mL deionized waters, after ultrasonic disperse 35min, added scattered The rare earth salt aqueous solution of agent neopelex and 7.5mol/mL, move into 100mL three-necked flask after ultrasonic disperse, After being warming up to 90 DEG C, mass concentration is added dropwise as 27wt% aqueous solution of urea 5mL using 0.6mL/min speed, drips off rear constant temperature 7h is reacted, is filtered, filter cake is washed with deionized, and is subsequently placed in 50 DEG C of thermostatic drying chamber and dries 12h, that is, is polymerize Thing/rare earth oxide complex microsphere, polymer/rare earth oxide complex microsphere is uniformly layered in crucible, crucible is put into horse Not calcined 4 hours at 850 DEG C in stove, rare earth oxide tiny balloon is obtained after being cooled to room temperature (25 DEG C, similarly hereinafter)；
(2) LBL self-assembly is handled
The rare earth oxide tiny balloon obtained in step (1) is soaked in the polyethylenimine solution that concentration is 3.5g/L 45min is steeped, 10min is rinsed under 0.5MPa pressure with deionized water after taking-up, is dried up；It is again that the rare earth oxide is hollow micro- Ball soaks 45min in the polyacrylic acid solution that concentration is 3.5g/L, and deionized water is used after taking-up in 0.5MPa pressure undershoot 10min is washed, is dried up, that is, completes double-deck deposition,
Repeat the above steps so that the number of plies of rare earth oxide tiny balloon adsorption deposition reaches 16 layers.
Each specific embodiment according to table 1 parts by weight match, by water-and acrylate, aqueous polyurethane, polysiloxanes, Doughnut, the rare earth oxide tiny balloon handled by LBL self-assembly, grapheme foam, bentonite use mechanical agitation Mode be well mixed, mixing speed is 180r/min under normal temperature, obtains vehicle environment protection damping material.
Table 1
Comparative example 1
Other any modifications such as LBL self-assembly are not carried out to rare earth oxide tiny balloon surface, remaining operation, component With embodiment 2.
Comparative example 2
Surface modification is carried out to rare earth oxide tiny balloon using the cladding means of other forms, remaining operation, component With embodiment 2：
(1) preparation of rare earth oxide tiny balloon
With embodiment 2；
(2) surface modification is handled
The rare earth oxide tiny balloon prepared in absolute ethyl alcohol, step (1), asphalt mixtures modified by epoxy resin are sequentially added into three-necked flask Fat E-44, triethylene tetramine and neopelex, after ultrasonic vibration 15min, flask is put into electric heating constant temperature water-bath In pot, at 40 DEG C after isothermal reaction 1h, temperature is raised to by 70 DEG C, and isothermal reaction 2h with 1 DEG C/min heating rate, whole During individual, the rotating speed of agitator maintains 1000rpm all the time；After reaction terminates, filtered product will be depressurized with anhydrous second Respectively the product after washing three times, is put into vacuum drying chamber, 12h is dried at 80 DEG C, that is, obtain organic epoxy by washing for alcohol, distilled water The rare earth oxide tiny balloon of resin solidification modification, and pass through the weight and reality of rate of charge control microsphere surface modification clad The gross weight for applying Iy self-assembled layer in example 2 is of substantially equal.
Formula of the microballoon after modification obtained above with reference to embodiment 2 in table 1 is prepared into vehicle environment protection damping material.
Comparative example 3
Only in LBL self-assembly operation, the number of plies for controlling rare earth oxide tiny balloon adsorption to deposit is 10 layers, Remaining operation, component are the same as embodiment 2.
The method of testing of the composite damping factor is as follows：Vehicle environment protection prepared by various embodiments above, comparative example is hindered Damping material pours into a long 21cm, wide 1cm, depth 3mm, bottom be placed with a 21cm*1cm*1mm steel spring plate tetrafluoro In ethene mould, by paste compaction, surface evening, after then drying 48 hours at room temperature, by the spring steel with damping material Plate takes out, and tests on the OBES damping factor testers of BK companies production and carries out, using simply supported beam test model,
The composite damping factor of damping material has damping when being 0.03, applies valency with reality during more than 0.05 Value, the composite damping factor shown in table 2 is primarily to characterize the vehicle environment protection damping material being prepared in real life In whether also there is damping.
Table 2

Claims (7)

  1. A kind of 1. novel vehicle graphene environmental-protection damp material, it is characterised in that：Described damping material is in parts by weight Including,
  2. 2. novel vehicle graphene environmental-protection damp material as claimed in claim 1, it is characterised in that：Described water soluble acrylic acid Ester is VN954, VN937, VN960, VN65, VN68, VN68S, VN710, VN605, VN610, VN650 or VN825.
  3. 3. novel vehicle graphene environmental-protection damp material as claimed in claim 1, it is characterised in that：Described aqueous polyurethane For AMS-2066,44V20, BC-6555, SP-90, BY-6555, PU-2890, QJ-6555, HK718, PU-3777A, IMK-800 Or PU-6011.
  4. 4. novel vehicle graphene environmental-protection damp material as claimed in claim 1, it is characterised in that：Described polysiloxanes is Amino-polyether polysiloxanes, saccharide-modified polyetherpolysilicone, polyurethane-polyether polysiloxane block copolymerized siloxanes, hexichol Ketone class polyetherpolysilicone or carboxy-modified polyetherpolysilicone.
  5. 5. novel vehicle graphene environmental-protection damp material as claimed in claim 1, it is characterised in that：Described process layer by layer from The preparation method of rare earth oxide tiny balloon for assembling processing is,
    (1) preparation of rare earth oxide tiny balloon
    Heated up after polymer emulsion, dispersant, rare earth salt aqueous solution are mixed, and aqueous solution of urea is added dropwise thereto, after dripping off Isothermal reaction, filter, dried after Washing of Filter Cake, that is, polymer/rare earth oxide complex microsphere is obtained, by polymer/rare earth oxygen Compound complex microsphere obtains rare earth oxide tiny balloon by calcining；
    (2) LBL self-assembly is handled
    The rare earth oxide tiny balloon obtained in step (1) is soaked in the solution of polyelectrolyte 1, rinses and blows after taking-up It is dry, then the rare earth oxide tiny balloon is soaked in the solution of polyelectrolyte 2, rinse and dry up after taking-up, that is, complete double-deck Deposition,
    Repeat the above steps, the number of plies for requiring rare earth oxide tiny balloon adsorption deposition.
  6. 6. novel vehicle graphene environmental-protection damp material as claimed in claim 5, it is characterised in that：Described polyelectrolyte 1 Or 2 be anion, cation or polyampholyte.
  7. 7. a kind of preparation method of novel vehicle graphene environmental-protection damp material as described in any one of claim 1 to 6, it is special Sign is：
    The preparation method is, by water-and acrylate, aqueous polyurethane, polysiloxanes, doughnut, by LBL self-assembly Rare earth oxide tiny balloon, grapheme foam, the bentonite of processing are well mixed.
CN201710804343.7A 2017-09-08 2017-09-08 A kind of novel vehicle graphene environmental-protection damp material and preparation method thereof Active CN107418110B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109177996A (en) * 2018-08-17 2019-01-11 中车青岛四方机车车辆股份有限公司 A kind of body construction of high-damping sound insulation composite material used for rail vehicle
CN109575736A (en) * 2018-07-05 2019-04-05 张家港市天源制漆涂装有限公司 A kind of graphene oxide damping paint and preparation method thereof based on flexible polymer modification

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JPH03146564A (en) * 1989-10-31 1991-06-21 Toyoda Gosei Co Ltd High damping material
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CN106893261A (en) * 2017-02-13 2017-06-27 中国船舶重工集团公司第七二五研究所 A kind of high-strength light porous metals composite damping material and preparation method thereof

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JPH03146564A (en) * 1989-10-31 1991-06-21 Toyoda Gosei Co Ltd High damping material
CN104194338A (en) * 2014-08-20 2014-12-10 南京信息工程大学 Environment-friendly rubber sound-insulation material and preparation method thereof
CN106893261A (en) * 2017-02-13 2017-06-27 中国船舶重工集团公司第七二五研究所 A kind of high-strength light porous metals composite damping material and preparation method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109575736A (en) * 2018-07-05 2019-04-05 张家港市天源制漆涂装有限公司 A kind of graphene oxide damping paint and preparation method thereof based on flexible polymer modification
CN109177996A (en) * 2018-08-17 2019-01-11 中车青岛四方机车车辆股份有限公司 A kind of body construction of high-damping sound insulation composite material used for rail vehicle

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