CN106496884A - A kind of carbon functional nano-composites and preparation method thereof - Google Patents
A kind of carbon functional nano-composites and preparation method thereof Download PDFInfo
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- CN106496884A CN106496884A CN201610909367.4A CN201610909367A CN106496884A CN 106496884 A CN106496884 A CN 106496884A CN 201610909367 A CN201610909367 A CN 201610909367A CN 106496884 A CN106496884 A CN 106496884A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention belongs to field of compound material, more particularly to a kind of carbon functional nano-composites and preparation method thereof.By CNT and Graphene, certain technique mix homogeneously makes carbon nanomaterial (mixture of CNT and Graphene) according to a certain percentage, and its surface is processed, eliminate or reduce the Van der Waals force between CNT and Coulomb force, improve their interface cohesions with rubber molecule, finally realize that carbon nanomaterial is dispersed in rubber, improve the combination property of rubber.Solving agglomeration traits, it is to avoid while dusting polluting environment, given play to CNT and Graphene advantage to the full extent, prepared high performance carbon nano-rubber product.
Description
Technical field
The invention belongs to field of compound material, more particularly to a kind of carbon functional nano-composites and preparation method thereof.
Background technology
Prior art be only single CNT or Graphene, related auxiliaries, rubber by internal mixer, open union
Machine or twin screw carry out mechanical blending, and CNT, Graphene still have serious reunion between other materials
Problem；Simultaneously as there is a problem of between the CNT or Graphene and rubber of inorganic material with reference to poor.
Problem above causes CNT or Graphene disperse well in rubber, can not give play to completely
The performance characteristics of oneself, show a lot of shortcomings on the contrary (such as hardness rise is fast, compression heat generation is obvious, intensity declines etc.).
Simultaneously CNT and Graphene be used as nano material, the characteristics of have itself again and difference.The benefit of CNT
Strong ability is eager to excel than Graphene, and ability of the Graphene in terms of conduction, heat conduction, radiating is more more advantageous than CNT.
But current way is essentially all that CNT and Graphene are isolated out use, and the group of also CNT and Graphene
Problem that is poly- serious and easily flying upward bad processing, causes to give a full play of its performance advantage, limits which and applies.Therefore, originally
Inventive concept is how CNT and Graphene to be combined performance, has complementary advantages, has given play to its advantage.
Content of the invention
The purpose of the present invention mainly fundamentally solves the reunion of CNT and the CNT as inorganic material
Combination problem with organic rubber material.
Technical scheme is as follows：
A kind of compositionss, are made up of the raw material of following weight portion：CNT 10-100 parts, Graphene 1-80 parts.
A kind of carbon functional nano-composites, its formula include combinations of the above thing, also include the raw material of following weight portion：
Rubber 10-100 parts, dispersant 0.2-20 parts, wetting agent 1-100 parts, softening agent 1-20 parts.
Preferably, other auxiliary agents of 1-20 parts are also included.
Preferably, the rubber is butadiene-styrene rubber, natural rubber, butadiene rubber, isoprene rubber, EP rubbers, butyl rubber
Glue, halogenated butyl rubber, nitrile rubber, hydrogenated nitrile-butadiene rubber, neoprene, ethylene-vinyl acetate rubber, polyurethane rubber
Glue, gutta-percha, gutta-percha, fluorubber, silicone rubber, chlorinated polyethylene rubber, CSM, butadiene-benzene second
Ethylenic thermoplastic elastomer, butadiene-styrene-vinyl cyanide thermoplastic elastomer (TPE), ethylene-propylene-esters of acrylic acid thermoplastic
The emulsion of at least one or above-mentioned rubber or elastomer in property elastomer, dispersion liquid, solution, monomer or performed polymer.
Preferably, the weight portion of the CNT is 30-60 parts.
Preferably, the weight portion of the Graphene is 25-60 parts.
Preferably, the composite is rubber master batch.
A kind of rubber master batch, its are prepared from by compositionss described above.
A kind of preparation method of carbon functional nano-composites, comprises the following steps：
1) first step
The surface preparation of carbon nanomaterial：CNT and Graphene are positioned over hermetic container according to aforementioned proportion
In, high-speed stirred is heated, dispersant high-temperature atomizing is added, CNT and graphenic surface cladding dispersant is made, is gradually cooled down
Cooling obtains the carbon nanomaterial being surface-treated；
Or CNT and Graphene are made aqueous solution according to a certain percentage, add dispersant, high-speed stirred or
Through being dried to obtain the mixture i.e. carbon nanomaterial of the CNT and Graphene that are coated with dispersant after ultrasound；
2) second step
By rubber, wetting agent, softening agent and other related auxiliaries in banbury mix homogeneously, then add above-mentioned carbon and receive
Rice material, according to rubber mixing technique intensification mix homogeneously, by the uniform rear bottom sheet of double roller open union machine bag roller mill, direct through comminutor
Pelletize obtains the material；
Or in hermetic container, under certain technique, intensification mixed at high speed is uniform by wetting agent and carbon nanomaterial, then
It is added in banbury together according to certain rubber mixing technique mix homogeneously, by double with rubber, softening agent, other related auxiliaries again
After roller bag roller is begun to pratise uniformly, bottom sheet obtains the material through granulator granulation；
Or RX and wetting agent and other related auxiliaries are added to intensification mix homogeneously in screw extruder
Afterwards, carbon nanomaterial is added to carry out being sufficiently mixed pelletize and obtain the material；
Or in hermetic container, under certain technique, intensification mixed at high speed is uniform by wetting agent and carbon nanomaterial, then
It is added in screw extruder together according to certain technique mix homogeneously, pelletize with rubber, softening agent and other related auxiliaries again
The composite is obtained, wherein softening agent includes liquid plasticizer, liquid rubber etc..
Preferably, the composite is rubber master batch.
The present invention Advantageous Effects be：By CNT and Graphene certain technique mix homogeneously according to a certain percentage
Carbon nanomaterial (mixture of CNT and Graphene) is made, and its surface is processed, eliminated or drop low-carbon nano
Van der Waals force and Coulomb force between pipe, fundamentally solves agglomeration traits；Introduce wetting agent to soak above-mentioned carbon nanomaterial
Profit, improves their interface cohesions with rubber molecule, finally realizes that carbon nanomaterial is dispersed in rubber, improves rubber
The combination property of product.Additionally, combining unique formula by the technique of mechanical blending produces the pre-dispersed rubber mother of carbon nanometer
Grain；Solve agglomeration traits, it is to avoid while dusting polluting environment, give play to the excellent of CNT and Graphene to the full extent
Gesture, prepares high performance carbon nano-rubber product.
Specific embodiment
Embodiment 1：The preparation of master batch
Raw material dosage：CNT and Graphene according to 20 1 ratios,
Fluorubber 50-60 parts, wetting agent 3-5 parts, softening agent (fluorosilicon oil) 2-5 parts, carbon nanomaterial 30-40 parts.
CNT and Graphene are placed into closed height according to a certain percentage to stir in machine, high-speed stirred intensification is carried out, are led to
Crossing batching hole adds dispersant to carry out atomization surface process, obtains surface-treated carbon nanomaterial after cooling.
Fluorubber, wetting agent and softening agent are added in banbury mixing is heated up uniformly according to certain rubber mixing technique,
Above-mentioned carbon nanomaterial is added, carries out again kneading uniform bottom sheet on banbury and open union machine according to certain technique, through pelletize
Machine pelletize, obtains high concentration carbon nanometer fluorubber pre-dispersing function master batch.Wherein softening agent includes liquid plasticizer, liquid rubber
Deng.
Embodiment 2：
Carbon nanometer fluorubber pre-dispersing function master batch in embodiment 1 is added to according to 10 parts, 20 parts, 30 parts, 40 parts
In llowing group of materials, the modified fluorubber sealing gasket vulcanizate of CNT predispersed masterbatch, specific performance such as table 1 is obtained：
Table 1
| Title material | 1# | 2# | 3# | 4# | 5# |
| 70 Mooney fluororubber of bis-phenol (morning twilight) | 100 | 94 | 88 | 82 | 76 |
| MgO-150 | 3 | 3 | 3 | 3 | 3 |
| Ca(OH)2 | 6 | 6 | 6 | 6 | 6 |
| WAX | 2 | 2 | 2 | 2 | 2 |
| CNT fluorubber pre-dispersing function master batch | 10 | 20 | 30 | 40 | |
| N990 | 20 | ||||
| AF | 2 | 2 | 2 | 2 | 2 |
| BPP | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Amount to | 133.5 | 117.5 | 121.5 | 125.5 | 129.5 |
Technical data
White carbon black is compared, is added CNT predispersed masterbatch and can be greatly improved the tensile strength of fluorubber and tear strong
Degree, while also retaining preferable percentage elongation, wearability is greatly improved, and the capacity of heat transmission is greatly improved, and is increased the service life.
Embodiment 3：
Carbon nanometer fluorubber pre-dispersing function master batch in embodiment 1 is added in llowing group of materials according to 8 parts, 12 parts,
Obtain the modified fluorubber sealing gasket vulcanizate of carbon nanometer predispersed masterbatch, specific performance such as table 2：
Table 2
| Title material | 1 | 2 | 3 |
| Fluorubber -70 (morning twilight) | 100 | 95.2 | 92.8 |
| MgO-150 | 3 | 3 | 3 |
| Ca(OH)2 | 6 | 6 | 6 |
| WAX | 2 | 2 | 2 |
| Carbon nanometer fluorubber pre-dispersing function master batch | 8 | 12 | |
| N990 | 20 | ||
| AF | 2 | 2 | 2 |
| BPP | 0.5 | 0.5 | 0.5 |
| Amount to | 133.5 | 120.8 | 124.5 |
Technical data
Compared with the fluorubber product of black-reinforced close with hardness, add CNT predispersed masterbatch can be lifted intensity and
Surely stretch, greatly improve wearability, while elevated temperature strength is substantially improved, extends the high temperature life of Fluororubber Seals, carry
High High temperature release safety.
Embodiment 4：
Raw material dosage：CNT and Graphene according to 20 1 ratios,
Nitrile rubber 40-55 parts, wetting agent 3-5 parts, softening agent (TP95) 10-15 parts, carbon nanomaterial 40-50 parts.
CNT and Graphene are placed into closed height according to a certain percentage to stir in machine, high-speed stirred intensification is carried out, are led to
Crossing batching hole adds dispersant to carry out atomization surface process, obtains surface-treated carbon nanomaterial after cooling.
Nitrile rubber, wetting agent, softening agent are added in banbury mixing is heated up uniformly according to certain rubber mixing technique,
Above-mentioned carbon nanomaterial is added, carries out again kneading uniform bottom sheet on banbury and open union machine according to certain technique, through pelletize
Machine pelletize, obtains high concentration carbon nanometer nitrile rubber pre-dispersing function master batch.Wherein softening agent includes liquid plasticizer, liquid rubber
Glue etc..
Described carbon nanometer nitrile rubber pre-dispersing function master batch is added to nitrile rubber according to 10 parts, 15 parts, 20 parts
100 parts, 5 parts of zinc oxide, 1 part of stearic acid, 2.5 parts of age resistor, 50 parts of white carbon black (N550), 10 parts of plasticizer (DOP), wax
(WB222) 2 parts, 0.4 part of Cosan, in the formula that 3.8 parts of accelerator, obtains the modified nitrile rubber of carbon nanometer predispersed masterbatch
Sealing gasket vulcanizate, specific performance such as table 3：
Table 3
Embodiment 5：
Raw material dosage：CNT and Graphene according to 20 1 ratios,
Ethylene propylene diene rubber 40-50 parts, wetting agent 3-5 parts, softening agent (paraffin oil) 8-12 parts, carbon nanomaterial 40-50
Part.
CNT and Graphene are placed into closed height according to a certain percentage to stir in machine, high-speed stirred are carried out and is warmed up to,
Add dispersant to carry out atomization surface process by batching hole, after cooling, obtain surface-treated carbon nanomaterial.
Ethylene propylene diene rubber, wetting agent, softening agent are added in banbury to heat up according to certain rubber mixing technique and are kneaded
Uniformly, above-mentioned carbon nanomaterial is added, carries out again kneading uniform bottom sheet on banbury and open union machine according to certain technique, passed through
Granulator granulation, obtains high concentration carbon nano ternary EP rubbers pre-dispersing function master batch.Wherein softening agent includes liquid plasticising
Agent, liquid rubber etc..
By carbon nano ternary EP rubbers pre-dispersing function master batch according to 0 part, 5 parts, 10 parts and 100 parts of ethylene-propylene-diene monomers
Glue, 87 parts of white carbon blacks, 15 parts of paraffin oil, 5 parts of zinc oxide, 1 part of age resistor, 3 parts of double 2,5 vulcanizing agents are according to certain technique in banburying
Machine, the mixing of open union machine obtain the modified EPT rubber packing pad vulcanizate of CNT predispersed masterbatch, and specific performance is such as
Table 4：
Table 4
Claims (10)
1. a kind of compositionss, it is characterised in that be made up of the raw material of following weight portion：CNT 10-100 parts, Graphene 1-
80 parts.
2. a kind of carbon functional nano-composites, it is characterised in that：Its formula includes the compositionss described in claim 1, also wraps
Include the raw material of following weight portion：Rubber 10-100 parts, dispersant 0.2-20 parts, wetting agent 1-100 parts, softening agent 1-20 parts.
3. a kind of carbon functional nano-composites as claimed in claim 2, it is characterised in that：Other for also including 1-20 parts are helped
Agent.
4. a kind of carbon functional nano-composites as claimed in claim 2, it is characterised in that：The rubber be butadiene-styrene rubber,
Natural rubber, butadiene rubber, isoprene rubber, EP rubbers, butyl rubber, halogenated butyl rubber, nitrile rubber, hydrogenated butyronitrile rubber
Glue, neoprene, ethylene-vinyl acetate rubber, polyurethane rubber, gutta-percha, gutta-percha, fluorubber, silicone rubber, chlorination
Polyethylene rubber, CSM, butadiene-styrene analog thermoplastic elastomer, butadiene-styrene-acrylonitrile
At least one or above-mentioned rubber or elastomer in analog thermoplastic elastomer, ethylene-propylene-Achievement of acrylate type thermo plastic elastomers
Emulsion, dispersion liquid, solution, monomer or performed polymer.
5. a kind of carbon functional nano-composites as claimed in claim 2, it is characterised in that：The weight portion of the CNT
For 30-60 parts.
6. a kind of carbon functional nano-composites as claimed in claim 2, it is characterised in that：The weight portion of the Graphene is
25-60 parts.
7. a kind of carbon functional nano-composites as claimed in claim 2, it is characterised in that：The composite is that rubber is female
Grain.
8. a kind of rubber master batch, it is characterised in that：Which is prepared from by the compositionss described in claim 1.
9. the preparation method of a kind of carbon functional nano-composites as described in any one of claim 2-7, it is characterised in that：Bag
Include following steps：
1) first step
The surface preparation of carbon nanomaterial：CNT and Graphene are positioned in hermetic container according to aforementioned proportion, plus
Hot high-speed stirred, adds dispersant high-temperature atomizing, makes CNT and graphenic surface cladding dispersant, gradually cools
Carbon nanomaterial to surface treatment；
Or CNT and Graphene are made aqueous solution according to a certain percentage, add dispersant, high-speed stirred or ultrasound
Afterwards through being dried to obtain the mixture i.e. carbon nanomaterial of the CNT and Graphene that are coated with dispersant；
2) second step
By rubber, wetting agent, softening agent and other related auxiliaries in banbury mix homogeneously, above-mentioned carbon nanometer material is then added
Material, according to rubber mixing technique intensification mix homogeneously, by the uniform rear bottom sheet of double roller open union machine bag roller mill, through the direct pelletize of comminutor
Obtain the material；
Or in hermetic container, under certain technique, intensification mixed at high speed is uniform by wetting agent and carbon nanomaterial, then again and
Rubber, softening agent, other related auxiliaries are added in banbury together according to certain rubber mixing technique mix homogeneously, by double roller bag
After roller is begun to pratise uniformly, bottom sheet obtains the material through granulator granulation；
Or RX and wetting agent and other related auxiliaries are added in screw extruder after intensification mix homogeneously, plus
Enter carbon nanomaterial and carry out being sufficiently mixed pelletize to obtain the material；
Or in hermetic container, under certain technique, intensification mixed at high speed is uniform by wetting agent and carbon nanomaterial, then again and
Rubber, softening agent and other related auxiliaries are added in screw extruder together according to certain technique mix homogeneously, and pelletize is obtained
The composite, wherein softening agent include liquid plasticizer, liquid rubber etc..
10. a kind of preparation method of carbon functional nano-composites as claimed in claim 9, it is characterised in that：Described compound
Material is rubber master batch.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163414A (en) * | 2017-06-23 | 2017-09-15 | 宁波艾克姆新材料有限公司 | A kind of graphene CBS is combined pre-dispersed masterbatch particles and preparation method thereof |
| CN107163469A (en) * | 2017-06-23 | 2017-09-15 | 宁波艾克姆新材料有限公司 | A kind of graphene DOTG is combined pre-dispersed masterbatch particles and preparation method thereof |
| CN107254107A (en) * | 2017-06-23 | 2017-10-17 | 宁波艾克姆新材料有限公司 | A kind of graphene MBI is combined pre-dispersed masterbatch particles and preparation method thereof |
| CN107955239A (en) * | 2017-11-29 | 2018-04-24 | 中国航发北京航空材料研究院 | The hydrogenated nitrile-butadiene rubber nanocomposite and preparation method of a kind of graphene-containing |
| CN108329609A (en) * | 2018-02-27 | 2018-07-27 | 合肥择浚电气设备有限公司 | A kind of high-strength Antistatic insulating material of heat-proof combustion-resistant and preparation method thereof |
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| WO2019011006A1 (en) * | 2017-07-12 | 2019-01-17 | 山东大展纳米材料有限公司 | Method and apparatus for preparing mixed rubber by continuous spray mixing |
| WO2021027345A1 (en) * | 2019-08-09 | 2021-02-18 | 湖北中澳纳米材料技术有限公司 | Nano-sized zinc molybdate production apparatus and method, and application thereof |
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| CN107163414A (en) * | 2017-06-23 | 2017-09-15 | 宁波艾克姆新材料有限公司 | A kind of graphene CBS is combined pre-dispersed masterbatch particles and preparation method thereof |
| CN107163469A (en) * | 2017-06-23 | 2017-09-15 | 宁波艾克姆新材料有限公司 | A kind of graphene DOTG is combined pre-dispersed masterbatch particles and preparation method thereof |
| CN107254107A (en) * | 2017-06-23 | 2017-10-17 | 宁波艾克姆新材料有限公司 | A kind of graphene MBI is combined pre-dispersed masterbatch particles and preparation method thereof |
| WO2019011006A1 (en) * | 2017-07-12 | 2019-01-17 | 山东大展纳米材料有限公司 | Method and apparatus for preparing mixed rubber by continuous spray mixing |
| CN107955239A (en) * | 2017-11-29 | 2018-04-24 | 中国航发北京航空材料研究院 | The hydrogenated nitrile-butadiene rubber nanocomposite and preparation method of a kind of graphene-containing |
| CN108329609A (en) * | 2018-02-27 | 2018-07-27 | 合肥择浚电气设备有限公司 | A kind of high-strength Antistatic insulating material of heat-proof combustion-resistant and preparation method thereof |
| CN108789458A (en) * | 2018-06-15 | 2018-11-13 | 中山米来机器人科技有限公司 | A kind of intelligent machine arm |
| WO2021027345A1 (en) * | 2019-08-09 | 2021-02-18 | 湖北中澳纳米材料技术有限公司 | Nano-sized zinc molybdate production apparatus and method, and application thereof |
| GB2600613A (en) * | 2019-08-09 | 2022-05-04 | Hubei Zhongao Nano Material Tech Co Ltd | Nano-sized zinc molybdate production apparatus and method, and application thereof |
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