CN106543739A - A kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material and preparation method thereof - Google Patents
A kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material and preparation method thereof Download PDFInfo
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- CN106543739A CN106543739A CN201610882263.9A CN201610882263A CN106543739A CN 106543739 A CN106543739 A CN 106543739A CN 201610882263 A CN201610882263 A CN 201610882263A CN 106543739 A CN106543739 A CN 106543739A
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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
- C08L87/00—Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C08L87/005—Block or graft polymers not provided for in groups C08L1/00 - C08L85/04
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The present invention discloses a kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material, is made up of the raw material of following weight portion：40 60 parts of nitrile rubber, 30 40 parts of chlorinated scoline, 128 160 parts of tetrahydrofuran, 42 61 parts of maleic anhydride, 26 parts of benzoyl peroxide, appropriate amount of ethanol, 13 parts of hydroxide sodium hypophosphite, appropriate dimethylbenzene, 24 33 parts of cork fibrous, 12 parts of stearic acid, 27 parts of white carbon black, 12 parts of sulfur, 47 parts of montmorillonite, 24 parts of hindered phenol HP1098, appropriate calcium chloride solution, appropriate deionized water.The present invention is grafted nitrile rubber using maleic anhydride, then compound with cork fibrous grafting, on the one hand strengthen the internal friction resistance of rubber molecular chain activity, the damping capacity of reinforcing material, on the other hand the sqouynd absorption lowering noise performance of damping material is improved using the characteristic of cork fibrous, prepare a kind of nitrile rubber damping material of damping noise reduction excellent performance.
Description
Technical field
The invention belongs to auto parts preparation field, and in particular to a kind of automobile hindered phenol/montmorillonite/nitrile rubber is multiple
Close damping material and preparation method thereof.
Background technology
Damping material is that a kind of material of damping noise reduction developed in recent years can be converted into heat vibration and acoustic energy
The new function material that can be dissipated, extensively applies in various plant equipment, front panel especially in the automobile seat room, car
There is application at the 8-12 position such as door, car roof, car bottom plate, boot, therefore researches and develops the new of excellent combination property
Efficient Damping material has become the focus of domestic and international concern.
What Tian Min, Lu Xun et al. were delivered《The preparation and performance study of blending type wide temperature zone high damping elastomeric material》One is literary
In, using having intensive pending methyl group, the chlorinated scoline of low pole to be blended with highly polar nitrile rubber in molecular structure, make
Binary CIIR/NBR blend is obtained, due to sterically hindered effect big in low pole rubber structure and the pressure after vulcanization crosslinking
Winding, it will increase the internal friction resistance of polar rubber strand activity, cause molecular chain movement to be obstructed, prepare wide temperature range
Damping material.
In nature, cork is a kind of very excellent material of damping performance, and it is the crust product of cork tree, is had
The performances such as good elasticity, sealing, heat-insulated, sound insulation, insulation, wear-resisting, corrosion resistance, protection against the tide, fire prevention, damping, can be used as ground
Plate, bottle stopper and woodwind instrument sealing gasket, packaging and energy absorbing material, heat-barrier material, damping damping material etc., are a kind of many work(
Can natural material.
Therefore, the present invention is grafted nitrile rubber using maleic anhydride, compounds with cork fibrous grafting then, on the one hand strengthens
On the other hand the internal friction resistance of rubber molecular chain activity, the damping capacity of reinforcing material is improved using the characteristic of cork fibrous
The sqouynd absorption lowering noise performance of damping material, prepares a kind of nitrile rubber damping material of damping noise reduction excellent performance.
The content of the invention
The invention aims to solve the problems, such as that existing damping material damping, sound absorbing capabilities are not enough, a kind of vapour is improved
Automobile-used hindered phenol/montmorillonite/nitrile rubber composite damping material and preparation method thereof.
A kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material, is made up of the raw material of following weight portion：
Nitrile rubber 40-60 parts, chlorinated scoline 30-40 parts, tetrahydrofuran 128-160 parts, maleic anhydride 42-61 parts, peroxidating
Benzoyl 2-6 parts, appropriate amount of ethanol, hydroxide sodium hypophosphite 1-3 parts, appropriate dimethylbenzene, cork fibrous 24-33 parts, stearic acid 1-2
Part, white carbon black 2-7 parts, sulfur 1-2 parts, montmorillonite 4-7 parts, hindered phenol HP1098 2-4 parts, appropriate calcium chloride solution, deionized water
In right amount.
Comprise the following steps that：
（1）Maleic anhydride is grafted nitrile rubber（MAH-g-NBR）Preparation：
Nitrile rubber is dissolved completely in tetrahydrofuran, maleic anhydride is added dropwise over benzoyl peroxide with Dropping funnel
Mixed solution, is passed through nitrogen protection, is warming up to 60-72 DEG C, and isothermal reaction 6-9 hours go out graft product with ethanol precipitation afterwards,
With washing with alcohol for several times, the graft product after washing is placed in 38-45 DEG C of vacuum drying oven and is dried, that is, obtain MAH-g-NBR,
It is standby；
（2）MAH-g-NBR is grafted cork fibrous：
Dimethylbenzene, hydroxide sodium hypophosphite and step are added in the boiling flask equipped with condensing tube（1）The MAH-g- for obtaining
NBR, afterwards by the abundant cork fibrous immersion mixed solution being dried, control temperature reacts 2-4 hours at 125-140 DEG C,
After the completion of reaction, solvent is removed with Soxhlet extractor, dried to constant weight in 95-105 DEG C, obtain final product MAH-g-NBR grafting corks fine
Dimension；
（3）The preparation of hindered phenol HP1098/ montmorillonite mixture：
In with the reaction bulb for continuing agitating device, sequentially add the pre-dispersed montmorillonite mixed liquor of deionized water, be obstructed
Phenol HP1098, it is coprecipitated to be stirring evenly and then adding into calcium chloride solution, using being dried after deionized water wash in an oven to constant weight, i.e.,
Obtain hindered phenol HP1098/ montmorillonite mixture；
（4）Mixing：
Under the conditions of 20-30 DEG C, by step（2）The MAH-g-NBR for obtaining is grafted cork fibrous, chlorinated scoline mix homogeneously
Plasticate on a mill 3-8 minutes, be subsequently adding stearic acid, white carbon black and step（3）The hindered phenol HP1098/ montmorillonites of preparation
Mixture kneads 10-30 minutes, adds sulfur mixing uniform afterwards, is prepared into elastomeric compound；
（5）Sulfuration：
By step（4）7-9 hours are stood after the thin pass-out piece of resulting elastomeric compound, on vulcanizing press at 160-190 DEG C
Hot press moulding vulcanizes 20-40 minutes, and hindered phenol/montmorillonite/nitrile rubber composite damping material is obtained.
Wherein, described cork fibrous are formed with the white softwood pulp plate mechanical dissociation of useless industrial source and dispersion, its length
Distribution 2mm-3.5mm, width distribution are 34.2 μm -73.1 μm, and length-width ratio is 72.6.
Compared with prior art, the present invention has advantages below：
（1）The present invention carries out graft modification first by maleic anhydride monomer to nitrile rubber, changes the polarity of nitrile rubber, increases
The internal friction resistance of additive polarity nitrile rubber strand activity, causes molecular chain movement to be obstructed, and molecule interchain frictional heat increases,
Damping capacity is more excellent.
（2）There are many gauffers on cork cell wall, can greatly alleviate compression, therefore elastic return is special
Good, the special cellularity of cork fibrous can weaken flat ripple and propagate in addition, enable in particular to the propagation of noise-reducing sound wave, thus soft
The sound absorption properties of wood utilizes this characteristic of cork fibrous very well in the present invention, be grafted nitrile rubber using maleic anhydride（MAH-g-
NBR）Cork fibrous are carried out with graft modification, the compatibility of the cork fibrous in rubber matrix is improved, subtracting for damping material is improved
Shake, sqouynd absorption lowering noise performance, can be effectively improved the comfort level of environment inside car, be conducive to the physical and mental health of people.
（3）Due to the huge surface area of montmorillonite, to small molecule phenols, amine etc. with good adsorption, this
Molten state hindered phenol is adsorbed in bright use montmorillonite, while strengthening polymer using its nano-lamellar structure also can to hindered phenol to
Surface migration plays interception, the premium properties such as the damping material of preparation has heat-resist, damping durability longer.
Specific embodiment
A kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material, is made up of the raw material of following weight portion：
Nitrile rubber 55, chlorinated scoline 35, tetrahydrofuran 157, maleic anhydride 58, benzoyl peroxide 4, appropriate amount of ethanol, hydrogen-oxygen
Change sodium hypophosphite 3, appropriate dimethylbenzene, cork fibrous 30, stearic acid 2, white carbon black 4, sulfur 2, montmorillonite 6, hindered phenol HP1098 3,
Appropriate calcium chloride solution, appropriate deionized water.
Comprise the following steps that：
（1）Maleic anhydride is grafted nitrile rubber（MAH-g-NBR）Preparation：
Nitrile rubber is dissolved completely in tetrahydrofuran, maleic anhydride is added dropwise over benzoyl peroxide with Dropping funnel
Mixed solution, is passed through nitrogen protection, is warming up to 70 DEG C, and isothermal reaction 8 hours goes out graft product with ethanol precipitation afterwards, uses second
Alcohol is washed for several times, the graft product after washing is placed in 40 DEG C of vacuum drying ovens and is dried, that is, obtain MAH-g-NBR, standby；
（2）MAH-g-NBR is grafted cork fibrous：
Dimethylbenzene, hydroxide sodium hypophosphite and step are added in the boiling flask equipped with condensing tube（1）The MAH-g- for obtaining
NBR, afterwards by the abundant cork fibrous immersion mixed solution being dried, control temperature is reacted 3 hours at 130 DEG C, has reacted
Cheng Hou, removes solvent with Soxhlet extractor, dries to constant weight in 100 DEG C, obtains final product MAH-g-NBR grafting cork fibrous；
（3）The preparation of hindered phenol HP1098/ montmorillonite mixture：
In with the reaction bulb for continuing agitating device, sequentially add the pre-dispersed montmorillonite mixed liquor of deionized water, be obstructed
Phenol HP1098, it is coprecipitated to be stirring evenly and then adding into calcium chloride solution, using being dried after deionized water wash in an oven to constant weight, i.e.,
Obtain hindered phenol HP1098/ montmorillonite mixture；
（4）Mixing：
Under the conditions of 20-30 DEG C, by step（2）The MAH-g-NBR for obtaining is grafted cork fibrous, chlorinated scoline mix homogeneously
Plasticate on a mill 7 minutes, be subsequently adding stearic acid, white carbon black and step（3）The hindered phenol HP1098/ montmorillonites of preparation are mixed
Compound is kneaded 25 minutes, is added sulfur mixing uniform afterwards, is prepared into elastomeric compound；
（5）Sulfuration：
By step（4）After the thin pass-out piece of resulting elastomeric compound stand 8 hours, on vulcanizing press at 170 DEG C high temperature mould
Pressure sulfuration 30 minutes, is obtained hindered phenol/montmorillonite/nitrile rubber composite damping material.
Wherein, described cork fibrous are formed with the white softwood pulp plate mechanical dissociation of useless industrial source and dispersion, its length
Distribution 2mm-3.5mm, width distribution are 34.2 μm -73.1 μm, and length-width ratio is 72.6.
Performance test：
Prepare according to embodiment and its material is tested, it is as a result as follows：
Density：1.192g/cm3, damping performance（23 DEG C, 200HZ）：0.16, fracture elongation：584%, tensile strength：
146Mpa, resistance to ag(e)ing：4 grades, light fastness aging：4 grades, roll processability：Well.
Claims (3)
1. a kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material, it is characterised in that by following weight portion
Raw material is constituted：Nitrile rubber 40-60 parts, chlorinated scoline 30-40 parts, tetrahydrofuran 128-160 parts, maleic anhydride 42-61
Part, benzoyl peroxide 2-6 parts, appropriate amount of ethanol, hydroxide sodium hypophosphite 1-3 parts, appropriate dimethylbenzene, cork fibrous 24-33 parts,
Stearic acid 1-2 parts, white carbon black 2-7 parts, sulfur 1-2 parts, montmorillonite 4-7 parts, hindered phenol HP1098 2-4 parts, calcium chloride solution are fitted
Amount, appropriate deionized water.
2. the preparation of the hindered phenol of a kind of automobile according to claims 1/montmorillonite/nitrile rubber composite damping material
Method, it is characterised in that comprise the following steps that：
（1）Maleic anhydride is grafted nitrile rubber（MAH-g-NBR）Preparation：
Nitrile rubber is dissolved completely in tetrahydrofuran, maleic anhydride is added dropwise over benzoyl peroxide with Dropping funnel
Mixed solution, is passed through nitrogen protection, is warming up to 60-72 DEG C, and isothermal reaction 6-9 hours go out graft product with ethanol precipitation afterwards,
With washing with alcohol for several times, the graft product after washing is placed in 38-45 DEG C of vacuum drying oven and is dried, that is, obtain MAH-g-NBR,
It is standby；
（2）MAH-g-NBR is grafted cork fibrous：
Dimethylbenzene, hydroxide sodium hypophosphite and step are added in the boiling flask equipped with condensing tube（1）The MAH-g- for obtaining
NBR, afterwards by the abundant cork fibrous immersion mixed solution being dried, control temperature reacts 2-4 hours at 125-140 DEG C,
After the completion of reaction, solvent is removed with Soxhlet extractor, dried to constant weight in 95-105 DEG C, obtain final product MAH-g-NBR grafting corks fine
Dimension；
（3）The preparation of hindered phenol HP1098/ montmorillonite mixture：
In with the reaction bulb for continuing agitating device, sequentially add the pre-dispersed montmorillonite mixed liquor of deionized water, be obstructed
Phenol HP1098, it is coprecipitated to be stirring evenly and then adding into calcium chloride solution, using being dried after deionized water wash in an oven to constant weight, i.e.,
Obtain hindered phenol HP1098/ montmorillonite mixture；
（4）Mixing：
Under the conditions of 20-30 DEG C, by step（2）The MAH-g-NBR for obtaining is grafted cork fibrous, chlorinated scoline mix homogeneously
Plasticate on a mill 3-8 minutes, be subsequently adding stearic acid, white carbon black and step（3）The hindered phenol HP1098/ montmorillonites of preparation
Mixture kneads 10-30 minutes, adds sulfur mixing uniform afterwards, is prepared into elastomeric compound；
（5）Sulfuration：
By step（4）7-9 hours are stood after the thin pass-out piece of resulting elastomeric compound, on vulcanizing press at 160-190 DEG C
Hot press moulding vulcanizes 20-40 minutes, and hindered phenol/montmorillonite/nitrile rubber composite damping material is obtained.
3. the system of the hindered phenol of a kind of automobile according to claims 1,2/montmorillonite/nitrile rubber composite damping material
Preparation Method, it is characterised in that described cork fibrous are formed with the white softwood pulp plate mechanical dissociation of useless industrial source and dispersion, its
Length distribution range 2mm-3.5mm, width distribution are 34.2 μm -73.1 μm, and length-width ratio is 72.6.
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| CN201610882263.9A CN106543739A (en) | 2016-10-10 | 2016-10-10 | A kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material and preparation method thereof |
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| CN201610882263.9A CN106543739A (en) | 2016-10-10 | 2016-10-10 | A kind of automobile hindered phenol/montmorillonite/nitrile rubber composite damping material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107698829A (en) * | 2017-10-11 | 2018-02-16 | 青岛科技大学 | A kind of wide temperature range damping rubber composite and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788836A (en) * | 2015-03-29 | 2015-07-22 | 安徽微威胶件集团有限公司 | Preparation method of high-damping rubber material |
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- 2016-10-10 CN CN201610882263.9A patent/CN106543739A/en not_active Withdrawn
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104788836A (en) * | 2015-03-29 | 2015-07-22 | 安徽微威胶件集团有限公司 | Preparation method of high-damping rubber material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107698829A (en) * | 2017-10-11 | 2018-02-16 | 青岛科技大学 | A kind of wide temperature range damping rubber composite and preparation method thereof |
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Application publication date: 20170329 |
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