CN109111605A - The preparation method and product of magnetorheological thermoplastic vulcanised elastomer damping material - Google Patents
The preparation method and product of magnetorheological thermoplastic vulcanised elastomer damping material Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/12—Making microcapsules or microballoons by phase separation removing solvent from the wall-forming material solution
- B01J13/125—Making microcapsules or microballoons by phase separation removing solvent from the wall-forming material solution by evaporation of the solvent
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- C08J2307/00—Characterised by the use of natural rubber
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/16—Ethene-propene or ethene-propene-diene copolymers
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/16—Ethene-propene or ethene-propene-diene copolymers
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The present invention relates to functional damping material technical fields, the preparation method and product of a kind of magnetorheological thermoplastic vulcanizates damping material are provided, which comprises the following steps: (1) preparation of nano magnetic material surface modification or magnetic fluid microcapsules;(2) preparation of nano magnetic material or magnetic fluid microcapsules and blend rubber system after modifying;(3) preparation of Rubber-Plastics Blends;(4) the pre- structuring of Rubber-Plastics Blends;(5) sulfidization molding of Rubber-Plastics Blends.Magnetorheological thermoplastic vulcanizates damping material prepared by the present invention is other than it can be avoided the problems such as magnetorheological fluid sedimentation, stability difference and magnetic liquid leak, also have many advantages, such as that controllability is good, magnetic response speed is fast, be not necessarily to encapsulation process, it can be widely applied to motor, machining, auto industry, the numerous areas such as medical treatment, therefore have a vast market application prospect.
Description
[technical field]
The present invention relates to functional damping material technical fields, and in particular to a kind of magnetorheological thermoplastic vulcanizates damping
The preparation method and product of material.
[background technique]
Magnetorheological materials are that intellectual material jumpy occurs for a kind of rheological property under the action of an external magnetic field, due to it
It is fast with response, good reversibility and can be by external magnetic field continuous control many advantages, such as, therefore be widely used in automobile,
Building, the numerous areas such as vibration control.
Magnetorheological fluid is presently the most common magnetorheological intellectual material, but it has the sedimentation of magnetic liquid in application process,
The problems such as stability is poor, and magnetic liquid leaks, is widely applied to limit it to a certain extent.Magnetic rheology elastic body is due to it
The advantages of having both magnetorheological materials and elastomer, and the sedimentation of magnetic liquid is overcome, the deficiencies of stability is poor, show huge answer
Use potentiality.
However traditional magnetic rheology elastic body is to be prepared later by vulcanization, using rubber as carrier although some materials
Practical application has been obtained, but since rubber material processing molding method itself is single, and is difficult to reuse after forming, from
And greatly limit its application.The unique phase structure of TPV and can is utilized in magnetorheological thermoplastic vulcanizate material
Repeat processing performance, can make its keep magneto-rheological characteristic and it is elastomeric simultaneously, and have good machine-shaping property
And the performances such as reusable, thus have broad application prospects and commercial value.
[summary of the invention]
The purpose of the present invention is to provide the preparation methods and production of a kind of magnetorheological thermoplastic vulcanised elastomer material
Product without encapsulation, and have good it is characterized in that having stability good using the magnetorheological elastomer material of this method preparation
Molding processibility and reusability.
In order to achieve the above-mentioned object of the invention, embodiments of the present invention provide a kind of magnetorheological thermoplastic vulcanizates bullet
The preparation method of property body damping material, comprises the following steps:
(1) preparation of nano magnetic material surface modification or magnetic fluid microcapsules: using coupling agent to nano-magnetic material
Material is surface modified or is prepared into the magnetic fluid microcapsule structure using resin as cyst wall, magnetic fluid base load liquid for core material;
(2) preparation of nano magnetic material or magnetic fluid microcapsules and blend rubber system after modifying: by receiving for modified
Rice magnetic material or magnetic fluid microcapsules are premixed with rubber phase, obtain magnetic particle/rubber or magnetic fluid microcapsules/rubber
Co-mixing system;
(3) preparation of Rubber-Plastics Blends: the co-mixing system that step (2) obtains is mixed with matrix resin, vulcanizing system
Uniformly, the rubber and plastic mixed system containing magnetic nanoparticle or magnetic fluid microcapsules is obtained;
(4) the pre- structuring of Rubber-Plastics Blends: the mixed system that step (3) obtains is filled into mold, magnetic is put into
Pre- structuring in thermal coupling vulcanization plant, obtaining magnetic nanoparticle in rubber phase or the magnetic particle in magnetic fluid microcapsules has
The pre- structured resin system of sequence arrangement;
(5) magnetic field, the pre- structured resin system sulphur that step (4) is obtained the sulfidization molding of Rubber-Plastics Blends: are closed
Change completely, obtains magnetorheological thermoplastic vulcanised elastomer material.
Preferably, nano magnetic material described in step (1) is metals, metal alloy or the metals such as iron, cobalt, nickel, manganese
At least one of oxide;The coupling agent be silane coupling agent, aluminate coupling agent and titanate coupling agent in extremely
Few one kind;And the dosage of the coupling agent is 0.5~3wt% of the heat filling.
Preferably, the cyst wall of magnetic fluid microcapsules described in step (1) is polypropylene, polyethylene, polyurethane, nylon
66, any in the organic polymers such as polymethyl acrylate, polycarbonate, ethylene propylene diene rubber, silicon rubber, acrylic rubber
It is a kind of;Base load liquid in the magnetic fluid microcapsules is metal or metal alloy or the metal oxide bases such as iron, cobalt, nickel, manganese
At least one of carrier fluid.
Preferably, rubber phase described in step (2) is ethylene propylene diene rubber, butyl rubber, nitrile rubber, acrylate
At least one of rubber, ethylene-acrylate rubber, ethylene octane copolymer, silicon rubber and fluorubber;The modified
Magnetic nanoparticle or magnetic fluid microcapsules and the mass ratio of the rubber phase are 50~300: 100.
Preferably, pre-compounding process described in step (2) carries out in mixer or open mill.
Preferably, matrix resin described in step (3) is polypropylene, polyethylene, polystyrene, polyamide, polychlorostyrene second
At least one of polymer such as alkene and polyurethane;The vulcanizing system is sulphur, peroxide, sulfur donor, metal
At least one of oxide and synthetic resin;The mass ratio of the co-mixing system and matrix resin, vulcanizing system is 100~50
: 70~50: 1.75~1.25.
Preferably, in the step (3), by co-mixing system and matrix resin, vulcanizing system be added double screw extruder or
It is uniformly mixed in open mill.
Preferably, in the magnetic-thermo coupling vulcanization plant in the step (4), magnetic field strength is 0.2~1T, temperature of heating plate
It is 25~200 DEG C.
Preferably, pre- structured resin system is vulcanized at 150~200 DEG C in step (5) completely.
Embodiments of the present invention also provide magnetorheological thermoplastic vulcanised elastomer prepared by the above method
Damping material, comprising matrix resin phase and the rubber phase being dispersed in described matrix resin phase, the rubber phase is to be modified
Magnetic material/blend rubber system is formed through externally-applied magnetic field sulfidization molding, and the modified magnetic material is the magnetic of coupling agent modification
Property nanoparticle or magnetic fluid microcapsules, and the modified magnetic material is uniformly distributed in the rubber phase.
Compared with the existing technology, magnetorheological thermoplastic vulcanised elastomer material provided by embodiments of the present invention
Material had both avoided the problems such as sedimentation of magnetic liquid present in magnetorheological fluid, stability are poor, and magnetic liquid leaks, and and had overcome magnetorheological rubber
Glue elastomer processing method is single, the not reproducible deficiency utilized, especially suitable for stable mass production and application, has wide
Wealthy market application prospect.
[Detailed description of the invention]
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing, in which:
Fig. 1 is the preparation flow schematic diagram of the magnetorheological thermoplastic vulcanised elastomer damping material in embodiment 1;
Fig. 2 is the preparation flow schematic diagram of the magnetorheological thermoplastic vulcanised elastomer damping material in embodiment 2.
[specific embodiment]
To make the object, technical solutions and advantages of the present invention clearer, below will to the embodiments of the present invention into
The detailed elaboration of row.However, it will be understood by those skilled in the art that in each embodiment of the present invention, in order to make to read
Person more fully understands the application and proposes many technical details.But even if without these technical details and based on following
The various changes and modifications of embodiment, each claim of the application technical solution claimed can also be realized.
In a specific embodiment of the invention, the system of magnetorheological thermoplastic vulcanised elastomer damping material is provided
Preparation Method comprises the following steps: (1) preparation of nano magnetic material surface modification or magnetic fluid microcapsules: utilizing coupling agent
Nano magnetic material is surface modified or is prepared into using resin as cyst wall, magnetic fluid base load liquid is the micro- glue of magnetic fluid of core material
Capsule structure;(2) preparation of nano magnetic material or magnetic fluid microcapsules and blend rubber system after modifying: by the nanometer of modified
Magnetic material or magnetic fluid microcapsules are premixed with rubber phase, obtain magnetic particle/rubber or magnetic fluid microcapsules/rubber is total
Mixed system;(3) preparation of Rubber-Plastics Blends: the co-mixing system that step (2) obtains is mixed with matrix resin, vulcanizing system
It is even, obtain the rubber and plastic mixed system containing magnetic nanoparticle or magnetic fluid microcapsules;(4) the pre- structuring of Rubber-Plastics Blends:
The mixed system that step (3) obtains is filled into mold, pre- structuring in magnetic-thermo coupling vulcanization plant is put into, obtains rubber phase
The pre- structured resin system of magnetic particle ordered arrangement in middle magnetic nanoparticle or magnetic fluid microcapsules;(5) rubber and plastic is total
The sulfidization molding of mixed system: closing magnetic field, and the pre- structured resin system that step (4) is obtained vulcanizes completely, obtains magnetorheological
Thermoplastic vulcanised elastomer material.
In a specific embodiment of the invention, nano magnetic material described in step (1) is the gold such as iron, cobalt, nickel, manganese
Category or at least one of metal alloy or metal oxide;The coupling agent be silane coupling agent, aluminate coupling agent and
At least one of titanate coupling agent;And the dosage of the coupling agent is 0.5~3wt% of the heat filling.
In a specific embodiment of the invention, the cyst wall of magnetic fluid microcapsules described in step (1) is polypropylene, gathers
Ethylene, polyurethane, nylon66 fiber, polymethyl acrylate, polycarbonate, ethylene propylene diene rubber, silicon rubber, acrylic rubber etc. have
Any one in machine polymer;Base load liquid in the magnetic fluid microcapsules is that the metals such as iron, cobalt, nickel, manganese or metal close
At least one of gold or metal oxide base load liquid.
In a specific embodiment of the invention, rubber phase described in step (2) is ethylene propylene diene rubber, butyl rubber
In glue, nitrile rubber, acrylic rubber, ethylene-acrylate rubber, ethylene octane copolymer, silicon rubber and fluorubber
It is at least one;The magnetic nanoparticle or magnetic fluid microcapsules of the modified and the mass ratio of the rubber phase are 50~300:
100。
In a specific embodiment of the invention, the pre-compounding process carries out in mixer or open mill.
In a specific embodiment of the invention, matrix resin described in step (3) is polypropylene, polyethylene, polyphenyl
At least one of polymer such as ethylene, polyamide, polyvinyl chloride and polyurethane;The vulcanizing system is sulphur, peroxidating
At least one of object, sulfur donor, metal oxide and synthetic resin;The co-mixing system and matrix resin, vulcanization body
The mass ratio of system is 100~50: 70~50: 1.75~1.25.
In a specific embodiment of the invention, in the step (3), by co-mixing system and matrix resin, vulcanizing system
It is added in double screw extruder or open mill and is uniformly mixed.
In a specific embodiment of the invention, in the magnetic-thermo coupling vulcanization plant in the step (4), magnetic field strength is
0.2~1T, temperature of heating plate are 25~200 DEG C.
In a specific embodiment of the invention, in step (5) by pre- structured resin system at 150~200 DEG C sulphur
Change complete.
A specific embodiment of the invention also provides magnetorheological thermoplastic vulcanizates bullet prepared by the above method
Property body damping material, comprising matrix resin phase and the rubber phase that is dispersed in described matrix resin phase, the rubber phase is
Modified magnetic material/blend rubber system is formed through externally-applied magnetic field sulfidization molding, and the modified magnetic material is coupling agent modification
Magnetic nano-particle or magnetic fluid microcapsules, and the modified magnetic material is uniformly distributed in the rubber phase.
It is some citings of a specific embodiment of the invention below:
Embodiment 1
(1) 100g carbonyl iron dust and 2g vinyltrimethoxysilane (silane coupling agent) coupling agent are dispersed respectively first
The ultrasonic disperse 1h in the mixed solution of dehydrated alcohol and a small amount of distilled water, mixes 1h at 70-80 DEG C for the two later, finally
Sample is dried into 6h in 70 DEG C of baking ovens, the magnetic material after being modified;
(2) the nano magnetic material 100g and 100g natural rubber of modified in (1) is placed in open mill and is premixed,
Obtain magnetic particle/blend rubber system;
(3) by magnetic particle/blend rubber system 200g in (2) and polypropylene 40g, (5g zinc oxide, 1g are hard for vulcanizing system
Resin acid, 3g sulphur) it is uniformly mixed in the open mill that roller temperature is 50-60 DEG C, obtain the rubber and plastic mixture containing magnetic nanoparticle
System.
(4) mixed system in (3) is filled into mold, being put into magnetic field strength is 0.8T, and temperature of heating plate is 150 DEG C
Magnetic-thermo coupling vulcanization plant in pre- structuring 20min, obtain the pre- structuring of magnetic nanoparticle ordered arrangement in rubber phase
Resin system.
(5) magnetic field is closed, the pre- structured resin system in (4) is vulcanized into 40min at 160 DEG C, obtains magnetic current heating
Plasticity vulcanised elastomer material.
The preparation flow figure of the present embodiment is as shown in Fig. 1.Magnetorheological thermoplastic vulcanizates obtained in the present embodiment
In elastomer damping material, include matrix resin phase and the rubber phase being dispersed in described matrix resin phase, the rubber
It is mutually that modified magnetic material/blend rubber system is formed through externally-applied magnetic field sulfidization molding, the modified magnetic material is coupling agent
The magnetic nano-particle or magnetic fluid microcapsules of modification, and the modified magnetic material is uniformly distributed in the rubber phase.
Embodiment 2
(1) 12g ethylene propylene diene rubber and 100g long chain alkane base load liquid system magnetic fluid are emulsified first, evaporation is made
Magnetic fluid microcapsules, and dried after being washed with distilled water;
(2) magnetic fluid microcapsules 100g and 100g ethylene propylene diene rubber in (1) is placed in open mill and is premixed, obtained
Magnetic fluid microcapsules/blend rubber system;
(3) by magnetic fluid microcapsules/blend rubber system 200g in (2) and polypropylene 40g, vulcanizing system (5g zinc oxide,
1g stearic acid, 3g octyl phenolic aldehyde) it is uniformly mixed in the open mill that roller temperature is 50-60 DEG C, obtain the rubber of the microcapsules containing magnetic fluid
Mould mixed system.
(4) mixed system in (3) is filled into mold, being put into magnetic field strength is 0.8T, and temperature of heating plate is 150 DEG C
Magnetic-thermo coupling vulcanization plant in pre- structuring 15min, obtain the pre- structuring of magnetic nanoparticle ordered arrangement in rubber phase
Resin system.
(5) magnetic field is closed, the pre- structured resin system in (4) is vulcanized into 30min at 160 DEG C, obtains magnetic current heating
Plasticity vulcanised elastomer material.
The preparation flow figure of the present embodiment is as shown in Fig. 2.Magnetorheological thermoplastic vulcanizates obtained in the present embodiment
In elastomer damping material, include matrix resin phase and the rubber phase being dispersed in described matrix resin phase, the rubber
It is mutually that modified magnetic material/blend rubber system is formed through externally-applied magnetic field sulfidization molding, the modified magnetic material is coupling agent
The magnetic nano-particle or magnetic fluid microcapsules of modification, and the modified magnetic material is uniformly distributed in the rubber phase.
It will be understood by those skilled in the art that the respective embodiments described above are to realize specific embodiments of the present invention,
And in practical applications, can to it, various changes can be made in the form and details, without departing from the spirit and scope of the present invention.
Claims (10)
1. a kind of preparation method of magnetorheological thermoplastic vulcanised elastomer damping material, which is characterized in that include following step
It is rapid:
(1) preparation of nano magnetic material surface modification or magnetic fluid microcapsules: using coupling agent to nano magnetic material into
Row surface modification is prepared into magnetic fluid microcapsule structure using resin as cyst wall, magnetic fluid base load liquid for core material;
(2) preparation of nano magnetic material or magnetic fluid microcapsules and blend rubber system after modifying: by the nano magnetic of modified
Property material or magnetic fluid microcapsules are premixed with rubber phase, obtain magnetic particle/rubber or magnetic fluid microcapsules/blend rubber
System;
(3) preparation of Rubber-Plastics Blends: the co-mixing system that step (2) obtains is uniformly mixed with matrix resin, vulcanizing system,
Obtain the rubber and plastic mixed system containing magnetic nanoparticle or magnetic fluid microcapsules;
(4) the pre- structuring of Rubber-Plastics Blends: the mixed system that step (3) obtains is filled into mold, magnetic thermal coupling is put into
Pre- structuring in vulcanization plant is closed, magnetic nanoparticle in rubber phase is obtained or the magnetic particle in magnetic fluid microcapsules is orderly arranged
The pre- structured resin system of column;
(5) sulfidization molding of Rubber-Plastics Blends: magnetic field is closed, the pre- structured resin system that step (4) obtains has been vulcanized
Entirely, magnetorheological thermoplastic vulcanised elastomer material is obtained.
2. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is,
Nano magnetic material described in step (1) be in metals, metal alloy or the metal oxide such as iron, cobalt, nickel, manganese extremely
Few one kind;
The coupling agent is at least one of silane coupling agent, aluminate coupling agent and titanate coupling agent;
And the dosage of the coupling agent is 0.5~3wt% of the nano magnetic material.
3. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is,
The cyst wall of magnetic fluid microcapsules described in step (1) is polypropylene, polyethylene, polyurethane, nylon66 fiber, polyacrylic acid first
Ester, polycarbonate, ethylene propylene diene rubber, silicon rubber, any one in acrylic rubber;
Base load liquid in the magnetic fluid microcapsules is iron, cobalt, nickel, manganese Metal, metal alloy or metal oxide base load liquid
At least one of.
4. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is,
Rubber phase described in step (2) is ethylene propylene diene rubber, butyl rubber, nitrile rubber, acrylic rubber, ethylene-
At least one of acrylic rubber, ethylene octane copolymer, silicon rubber and fluorubber;
The nano magnetic material or magnetic fluid microcapsules of the modified and the mass ratio of the rubber phase are 50~300: 100.
5. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is, pre-compounding process described in step (2) carries out in mixer or open mill.
6. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is,
Matrix resin described in step (3) is polypropylene, polyethylene, polystyrene, polyamide, polyvinyl chloride and polyurethane etc.
At least one of polymer;
The vulcanizing system is at least one in sulphur, peroxide, sulfur donor, metal oxide and synthetic resin
Kind;
The mass ratio of the co-mixing system and matrix resin, vulcanizing system is 100~50: 70~50: 1.75~1.25.
7. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is, in the step (3), co-mixing system and matrix resin, vulcanizing system is added in double screw extruder or open mill and is mixed
It closes uniform.
8. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is, in the magnetic-thermo coupling vulcanization plant in the step (4), magnetic field strength is 0.2~1T, and temperature of heating plate is 25~200
℃。
9. the preparation method of magnetorheological thermoplastic vulcanised elastomer damping material according to claim 1, feature
It is, vulcanizes pre- structured resin system completely at 150~200 DEG C in step (5).
10. the magnetorheological thermoplastic vulcanised elastomer damping that method described in any one of claims 1 to 9 is prepared
Material includes matrix resin phase and the rubber phase being dispersed in described matrix resin phase, which is characterized in that
The rubber phase is that modified magnetic material/blend rubber system is formed through externally-applied magnetic field sulfidization molding, the modified magnetic
Material is the magnetic Nano material or magnetic fluid microcapsules of coupling agent modification, and the modified magnetic material is in the rubber phase
It is uniformly distributed.
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