CN101974179A - High-conductivity composite material and preparation method thereof - Google Patents
High-conductivity composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-conductivity composite material and a preparation method thereof. The high-conductivity nano composite material comprises a crystalline polymer, a carbon nano tube and an organic nucleating agent of the crystalline polymer. The preparation method comprises the following steps: mixing the three raw materials in a dimethylbenzene solvent according to a proper proportion and order; and volatizing the solvent under a continuous ultrasonic condition to obtain the high-conductivity composite material. The method is simple and easy to operate and can obtain the conductive composite material with high conductivity and comprehensive performance through a simple way; and the composite material can be widely applied to the fields of automobiles, electronics and electronic instrument, office equipment, industrial machinery and the like, and meet and expand the application of the crystalline high polymer material in the fields of conductive material, electromagnetic shielding and the like.
Description
Technical field
The present invention relates to a kind of high conductivity matrix material and preparation method thereof, particularly, relate to crystal polymer thing/carbon nano tube compound material, belong to polymer-based composite preparation and carbon nano-tube modification field.
Background technology
Carbon nanotube suddenly becomes the focus of Chinese scholars research owing to machinery, calorifics and electric property with excellence and uniqueness.In recent years, in the industrial production of reality, carbon nanotube is owing to its volume production small scale, the factor that limits its widespread use that becomes with high costs; In the carbon nanotubes reinforced polymer based composites, because the effect of the Van der Waals force between the carbon nanotube tube wall, peeling off and disperseing the consistency of back in matrix of carbon nano-tube bundle is the key point of preparation carbon nano tube compound material.Therefore, the modification of carbon nanotube has important use value for its good distribution and interface compatibility in polymkeric substance.
The functionalization research method of carbon current nanotube mainly contains covalent modification and two aspects of non covalent bond modification.Covalent modification is exactly that the functionalization group directly is keyed to the surface of carbon pipe or the defective locations on the carbon tube-surface, also can superscribe the firm polymer layer of one deck in carbon nano tube surface by home position polymerization reaction, at Chemistry Materials in 2005, in 1290～1295 pages of reports of 17 volumes: by means of H
2SO
4/ HNO
3Mixed acid solution is handled carbon nanotube (CNTs), obtain the modified carbon nano-tube that the surface has carboxyl, can carry out a series of chemically modified to introduce different functional groups to carboxyl subsequently, covalent modification has destroyed the structure of carbon nanotube to a certain extent, the reduction that this has just caused the mechanics and the electric property of carbon nanotube has influenced the performance of its performance in matrix material.The non covalent bond modification then is to adopt tensio-active agent, oligopolymer or inorganic functional molecule that carbon nanotube is carried out the physical adsorption modification, on the one hand to strengthen its solubility, can improve its consistency in matrix on the one hand in addition, also influence some character of matrix simultaneously.Journal of American Chemistry Society in 2006, π-πGong Ezuoyong a little less than 128 volumes 1692～1699 have been introduced between the tube wall graphite-structure that the non covalent bond method for coating will have the small molecules of aromatic nucleus or polymkeric substance and carbon nanotube is introduced some active groups.The present invention adopts fragrant same clan organic nucleating agent non covalent bond carbon nano-tube modified, both can guarantee to improve dispersiveness and the consistency of carbon nanotube in matrix under the prerequisite that carbon nanotube structure is not destroyed, by the influence of organic nucleating agent to the matrix crystallisation process, the size in control crystallite district realizes the optimization of carbon nano tube network simultaneously.
Summary of the invention
At above problems of the prior art, the objective of the invention is to propose that a kind of material property is good, the simple carbon nanotube composite modification material of recombining process and preparation method thereof.
The carbon nanotube composite modification material that the present invention proposes, finishing at carbon nanotube, utilize aromatic organic nucleating agent to come modified carbon nano-tube, by π-πGong Ezuoyong it is adsorbed onto carbon nano tube surface, not only can improve the dispersiveness of carbon nanotube in solution, strengthen the consistency between carbon nanotube and crystal polymer thing, and organic nucleating agent can be by the crystallisation process of impact polymer, comprise crystalline crystalline region size, arrange and crystal formation waits and optimizes carbon nanotube network, it is low to prepare cost, comprehensive physics good mechanical property, crystal polymer thing/the carbon nano tube compound material that conducts electricity very well.
Technical scheme of the present invention is as follows:
A kind of high conductivity matrix material that the present invention proposes is characterized in that, comprises 94.0～99.4% crystal polymer thing, 0.5～5.0% carbon nanotube and 0.1～1.0% organic nucleating agent.
Described crystal polymer thing is selected from polypropylene (PP) or polymeric amide.
Described carbon nanotube is Single Walled Carbon Nanotube, double-walled carbon nano-tube or multi-walled carbon nano-tubes.
Described organic nucleating agent adopts two [4-(1,1-dimethyl ethyl) benzoyl-oxygen] aluminium hydroxide of aryl dicarboxylic acid's acid amides, the benzoyl class of aryl class, and its chemical structural formula is shown below respectively:
Act as non covalent bond π-pi-conjugated adsorption between described organic nucleating agent and the described carbon nanotube.
The preparation method of described high conductivity nano composite material comprises the steps:
A) o-dichlorobenzene solution of configuration carbon nanotube-organic nucleating agent: carbon nanotube and organic nucleating agent are added in orthodichlorobenzene or the perhydronaphthalene, ultra-sonic dispersion 40～120min under 15～45 ℃ of environment, the concentration of the carbon nanotube-orthodichlorobenzene of configuration or perhydronaphthalene solution (with the volumeter of quality in the carbon nanotube and orthodichlorobenzene or perhydronaphthalene) is 0.1～1.0 mg/ml;
B) solution after ultrasonic is placed 0 ℃ ice-water bath 0.5～1.0 h after, use the aperture to continue under 0 ℃ environment, to filter at the filter paper of 0.45 μ m, on filter paper, obtained the organic nucleating agent modified carbon nanotube like this.At last modified carbon nanotube is dispersed in again in the solvent (as toluene or dimethylbenzene), ultra-sonic dispersion 0.5～1.0 h obtains the carbon nano-tube solution that stable organic nucleating agent is modified;
C) carbon nano-tube solution that the organic nucleating agent for preparing in the step b) is modified dropwise is added drop-wise in the hot solution (110～150 ℃) that is dissolved with the crystal polymer thing, again system is remained in continue in 110～150 ℃ the environment ultrasonic until most solvent evaporates;
D) take out final product in the step c), be positioned over 12～24h in 90 ℃ the vacuum drying oven, so just obtain finishing crystal formation polymer/carbon nano-tube matrix material.
Described carbon nanotube is Single Walled Carbon Nanotube, double-walled carbon nano-tube or multi-walled carbon nano-tubes.
The consumption of described organic nucleating agent is 0.1～1.0% of a crystal polymer amount.
Has following outstanding advantage by the conducing composite material of use present method preparation and traditional polymer/carbon nano-tube matrix material: by in crystal polymer thing/carbon nano tube compound material, adding organic nucleating agent non covalent bond modified carbon nanotube, the crystal polymer thing there is following influence: 1) change the polymer crystallization degree, because carbon nanotube can only be present in the amorphous portion in the crystal polymer thing, so this can change the effective volume that carbon nanotube distributes in the crystal polymer thing; 2) organic nucleating agent is adsorbed on carbon nano tube surface by the non covalent bond mode and helps improving the dispersion of carbon nanotube in matrix; 3) effectively improve interface binding power between carbon nanotube and the crystal polymer thing; 4) influence the crystallization behavior of crystal polymer thing, grain refining helps carbon nanotube arranging in polymkeric substance, can increase substantially the electric conductivity of matrix material, and specific conductivity reaches 10
-2S/cm.And because the consumption of carbon nanotube seldom reaches the existence of beta crystal in the matrix material, can also keep the elongation at break of polymkeric substance, thereby reach the purpose for preparing high conductivity composite material with low cost, have important academic significance and using value.
Description of drawings
Fig. 1 is the field emission scanning electron microscope figure of embodiment 1 crystal polymer thing/organic beta nucleater carbon nano-tube modified (5.0wt) matrix material.
Fig. 2 is the field emission scanning electron microscope figure of embodiment 4 crystal polymer things/organic α nucleator carbon nano-tube modified (5.0wt) matrix material.
Embodiment
Below by embodiment the present invention is specifically described.Be necessary to be pointed out that at this following examples only are used for that the invention will be further described; can not be interpreted as limiting the scope of the invention; some nonessential improvement and adjustment that the professional and technical personnel in this field content according to the present invention is made still belong to protection scope of the present invention.
Embodiment 1
1) with 5.0wt% multi-walled carbon nano-tubes and the organic beta nucleater of 0.75wt%---aryl dicarboxylic acid's acid amides of aryl class joins in the round-bottomed flask that the 100ml orthodichlorobenzene is housed, in 0 ℃ ice-water bath, leave standstill 0.5h behind the supersound process 2h under the room temperature, keep under this temperature with 0.22 μ m filtering with microporous membrane, obtain the organic beta nucleater modified multi-walled carbon nano-tubes of 0.10wt% content, its ultra-sonic dispersion is being obtained dispersion liquid in xylene solvent;
2) taking by weighing the 94.9wt% polypropylene is dissolved under stirring environment in 140 ℃ the xylene solvent, afterwards with 1) in dispersant liquid drop add in the so far hot dimethylbenzene, continue ultrasonic 3h to most xylene solution volatilization;
3) with 2) in the product that obtains place 90 ℃ vacuum drying oven vacuum-drying 24h.Obtain the aryl dicarboxylic acid's acid amides modified carbon nanotube/polyacrylic matrix material of aryl class.
Fig. 1 is the field emission scanning electron microscope figure of this embodiment product crystal polymer thing/organic beta nucleater carbon nano-tube modified (5.0wt) matrix material.
Embodiment 2
1) with 5.0wt% multi-walled carbon nano-tubes and the organic beta nucleater of 1.65wt%---aryl dicarboxylic acid's acid amides of aryl class joins in the round-bottomed flask that the 100ml orthodichlorobenzene is housed, in 0 ℃ ice-water bath, leave standstill 0.5h behind the supersound process 2h under the room temperature, keep under this temperature with 0.45 μ m filtering with microporous membrane, obtain the organic beta nucleater modified multi-walled carbon nano-tubes of 1.0wt% content, its ultra-sonic dispersion is being obtained dispersion liquid in toluene solvant;
2) taking by weighing the 94.0wt% polypropylene is dissolved under stirring environment in 140 ℃ the toluene solvant, afterwards with 1) in dispersant liquid drop add so far in the hot toluene, continue ultrasonic 3h to most toluene solution volatilization;
3) with 2) in the product that obtains place 120 ℃ vacuum drying oven vacuum-drying 24h.Obtain the aryl dicarboxylic acid's acid amides modified carbon nanotube/polyacrylic matrix material of aryl class.
Embodiment 3
1) with 0.5wt% multi-walled carbon nano-tubes and the organic beta nucleater of 0.75wt%---aryl dicarboxylic acid's acid amides of aryl class joins in the round-bottomed flask that the 100ml orthodichlorobenzene is housed, in 0 ℃ ice-water bath, leave standstill 0.5h behind the supersound process 2h under the room temperature, keep under this temperature with 0.45 μ m filtering with microporous membrane, obtain the organic beta nucleater modified multi-walled carbon nano-tubes of 0.1wt% content, its ultra-sonic dispersion is being obtained dispersion liquid in toluene solvant;
2) taking by weighing the 99.4wt% polypropylene is dissolved under stirring environment in 140 ℃ the toluene solvant, afterwards with 1) in dispersant liquid drop add so far in the hot toluene, continue ultrasonic 3h to most toluene solution volatilization;
3) with 2) in the product that obtains place 120 ℃ vacuum drying oven vacuum-drying 24h.Obtain the aryl dicarboxylic acid's acid amides modified carbon nanotube/polyacrylic matrix material of aryl class.
Embodiment 4
1) with 5.0wt% multi-walled carbon nano-tubes and the organic α nucleator of 0.75wt%---two [4-(1 of benzoyl class, the 1-dimethyl ethyl) benzoyl-oxygen] aluminium hydroxide joins in the round-bottomed flask that the 100ml orthodichlorobenzene is housed, in 0 ℃ ice-water bath, leave standstill 0.5h behind the supersound process 2h under the room temperature, keep under this temperature with 0.22 μ m filtering with microporous membrane, obtain the nucleater modified multi-walled carbon nano-tubes of organic α of 0.10wt% content, its ultra-sonic dispersion is being obtained dispersion liquid in xylene solvent;
2) taking by weighing the 94.9wt% polypropylene is dissolved under stirring environment in 140 ℃ the xylene solvent, afterwards with 1) in dispersant liquid drop add in the so far hot dimethylbenzene, continue ultrasonic 3h to most xylene solution volatilization;
3) with 2) in the product that obtains place 90 ℃ vacuum drying oven vacuum-drying 24h.Obtain the aryl dicarboxylic acid's acid amides modified carbon nanotube/polyacrylic matrix material of aryl class
Fig. 2 is the field emission scanning electron microscope figure of this embodiment product crystal polymer thing/organic α nucleator carbon nano-tube modified (5.0wt) matrix material.
Embodiment 5
1) with 2.0wt% multi-walled carbon nano-tubes and the organic beta nucleater of 0.75wt%---aryl dicarboxylic acid's acid amides of aryl class joins in the round-bottomed flask that the 100ml orthodichlorobenzene is housed, in 0 ℃ ice-water bath, leave standstill 0.5h behind the supersound process 2h under the room temperature, keep under this temperature with 0.45 μ m filtering with microporous membrane, obtain the organic beta nucleater modified multi-walled carbon nano-tubes of 0.1wt% content, its ultra-sonic dispersion is being obtained dispersion liquid in toluene solvant;
2) taking by weighing the 99.4wt% polypropylene is dissolved under stirring environment in 140 ℃ the toluene solvant, afterwards with 1) in dispersant liquid drop add so far in the hot toluene, continue ultrasonic 3h to most toluene solution volatilization;
3) with 2) in the product that obtains place 120 ℃ vacuum drying oven vacuum-drying 24h.Obtain the aryl dicarboxylic acid's acid amides modified carbon nanotube/polyacrylic matrix material of aryl class.
Above-mentioned carbon nanotube can also be single wall or double-walled.
Following table 1 is the specific conductivity of the carbon nano tube compound material of crystal polymer thing of the present invention/organic nucleating agent modification.
Table 1
The present invention carries out compound method so simply and effectively by the organic nucleating agent with crystal polymer thing, carbon nanotube and crystal polymer thing, just can obtain the matrix material of good conductivity.In the prepared crystal polymer thing/carbon nanotube conducting nano composite material that goes out: the organic nucleating agent of crystal polymer thing has not only played dispersing Nano carbon tubes in solvent and the effect in the matrix, also improved simultaneously the consistency between carbon nanotube and the matrix, outstanding more is that it has influenced the crystal property of crystal type polymkeric substance and the character of crystallizing field, makes carbon nanotube form more effectively conductive network like this.Therefore, this law help preparing that low, the comprehensive physical and mechanical properties of cost is good, all good carbon nanotube/crystal polymer thing nano composite materials of conductivity.
Claims (8)
1. a high conductivity nano composite material is characterized in that, comprises the component that following weight percent is represented: 94.0～99.4% crystal polymer thing, 0.5～5.0% carbon nanotube and 0.1～1.0% organic nucleating agent.
2. high conductivity nano composite material according to claim 1 is characterized in that, described crystal polymer thing is selected from polypropylene or polymeric amide.
3. high conductivity nano composite material according to claim 1 is characterized in that, described carbon nanotube adopts Single Walled Carbon Nanotube, double-walled carbon nano-tube or multi-walled carbon nano-tubes.
4. high conductivity nano composite material according to claim 1, it is characterized in that, described organic nucleating agent adopts two [4-(1,1-dimethyl ethyl) benzoyl-oxygen] aluminium hydroxide of aryl dicarboxylic acid's acid amides, the benzoyl class of aryl class, and its chemical structural formula is shown below respectively.
5. according to claim 1 or 4 described high conductivity nano composite materials, it is characterized in that, act as non covalent bond π-pi-conjugated adsorption between described organic nucleating agent and the described carbon nanotube.
6. the preparation method of the high conductivity nano composite material of claim 1 is characterized in that, comprises the steps:
A) o-dichlorobenzene solution of configuration carbon nanotube-organic nucleating agent: carbon nanotube and organic nucleating agent are added in orthodichlorobenzene (DCB) or the perhydronaphthalene ultra-sonic dispersion 40～120min under 15～45 ℃ of environment;
With the quality of carbon nanotube and the volumeter of orthodichlorobenzene, the concentration of the orthodichlorobenzene of the carbon nanotube-organic nucleating agent of configuration or perhydronaphthalene solution is 0.1～1.0 mg/ml;
B) o-dichlorobenzene solution after ultrasonic is placed 0 ℃ ice-water bath 0.5～1.0 h after, the use aperture is that the porous membrane of 0.22 μ m～0.45 μ m continues to filter under 0 ℃ environment, has obtained described organic nucleating agent modified carbon nanotube on porous membrane; At last described modified carbon nanotube is dispersed in the solvent again, ultra-sonic dispersion 0.5～1.0 h in the ultrasonic pond obtains stable modified carbon nano-tube solution;
C) described modified carbon nano-tube solution dropwise being added drop-wise to the temperature that is dissolved with the crystal polymer thing is in 110～150 ℃ the hot solution, then system is remained in that to use ultrasonic probe to continue in 110～150 ℃ the environment ultrasonic until most solvent evaporates;
D) take out final product in the step c), be positioned over 12～24h in 80～120 ℃ the vacuum drying oven, obtain the matrix material of carbon nanotube/crystal polymer thing;
Described carbon nanotube is Single Walled Carbon Nanotube, double-walled carbon nano-tube or multi-walled carbon nano-tubes.
7. preparation method according to claim 6 is characterized in that, the consumption of described organic nucleating agent is 0.1～1.0% of a crystal polymer amount.
8. preparation method according to claim 6 is characterized in that, described solvent is dimethylbenzene or toluene.
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| CN102675893A (en) * | 2012-06-04 | 2012-09-19 | 西南交通大学 | Method for preparing polymer-based conducting composite material by melt blending |
| CN102888092A (en) * | 2012-02-01 | 2013-01-23 | 厦门长塑实业有限公司 | Quickly crystallized nylon compound and preparation method thereof |
| CN105482244A (en) * | 2014-10-11 | 2016-04-13 | 中国石油化工股份有限公司 | Carbon nano-tube/polymer composite material and preparation method thereof |
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| CN102888092B (en) * | 2012-02-01 | 2014-04-23 | 厦门长塑实业有限公司 | Quickly crystallized nylon compound and preparation method thereof |
| CN102675893B (en) * | 2012-06-04 | 2014-07-02 | 西南交通大学 | Method for preparing polymer-based conducting composite material by melt blending |
| CN102675893A (en) * | 2012-06-04 | 2012-09-19 | 西南交通大学 | Method for preparing polymer-based conducting composite material by melt blending |
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| CN105482244B (en) * | 2014-10-11 | 2019-05-31 | 中国石油化工股份有限公司 | A kind of carbon nano-tube/polymer composite material and preparation method thereof |
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| CN105693968B (en) * | 2016-02-02 | 2018-09-25 | 宁波西博恩新材料科技有限公司 | High performance polyurethane buffering composite material based on Nano filling and preparation method thereof |
| CN105693977B (en) * | 2016-02-02 | 2018-09-25 | 宁波西博恩新材料科技有限公司 | High performance polyurethane energy-absorbing composite material and preparation method based on Nano filling |
| CN105693977A (en) * | 2016-02-02 | 2016-06-22 | 宁波西博恩新材料科技有限公司 | Nano-filler-based high-performance polyurethane energy-absorption composite material and preparation method thereof |
| CN106633391A (en) * | 2016-11-29 | 2017-05-10 | 华东理工大学 | Inducing method of transcrystalline structure on polypropylene/glass fiber interface |
| WO2019159025A1 (en) * | 2018-02-14 | 2019-08-22 | International Business Machines Corporation | A crystalline film of carbon nanotubes |
| CN111655366A (en) * | 2018-02-14 | 2020-09-11 | 国际商业机器公司 | Carbon nanotube crystal sheet |
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Application publication date: 20110216 |