CN101418089A - Method for preparing natural rubber-carbon nano tube composite material by using static electricity self-assembly - Google Patents
Method for preparing natural rubber-carbon nano tube composite material by using static electricity self-assembly Download PDFInfo
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- CN101418089A CN101418089A CNA2008102279752A CN200810227975A CN101418089A CN 101418089 A CN101418089 A CN 101418089A CN A2008102279752 A CNA2008102279752 A CN A2008102279752A CN 200810227975 A CN200810227975 A CN 200810227975A CN 101418089 A CN101418089 A CN 101418089A
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Abstract
The invention provides a method for utilizing electrostatic self-assembly to prepare a natural rubber-carbon nano-tube composite material. The method comprises the following steps of adopting surfactant to modify the surfaces of carbon nano-tubes so as to enable the surfaces of the carbon nano-tubes to have positive charges, directly mixing the carbon nano-tubes with lacteous natural rubber with negative charges and utilizing self-assembly in an electrostatic adsorption principle to prepare the natural rubber-carbon nano-tube composite material. The preparation method realizes that the carbon nano-tubes are uniformly dispersed in the natural rubber and have good compatibility with the natural rubber, thereby providing technical guarantee for preparing nano-composite rubber products with excellent comprehensive properties.
Description
[invention field]
The present invention relates to the preparation method of native rubber composite material, particularly a kind of preparation method who utilizes the static self-assembly to prepare natural rubber-carbon nano tube composite material.
[background technology]
Carbon nanotube is just found a kind of novel carbon structure in 1991, and it is seamless, the hollow tube body that is rolled into by the Graphene lamella that carbon atom forms.Because the radial dimension of carbon nanotube is very little, the diameter of pipe generally in several nanometers to tens nanometers, and the length of carbon nanotube is generally at several microns to tens microns, so carbon nanotube is considered to a kind of typical monodimension nanometer material.Carbon nanotube has excellent mechanical property, and tensile strength reaches 50GPa～200GPa, be approximately 100 times of steel, and density has only the sixth of steel.The axial thermal conductivity that carbon nanotube is also good just like chemical stability in addition, thermostability is high, good, low-temperature superconducting, electromaganic wave absorbing property and many performances such as adsorptivity preferably are the ideal fillers of polymer composites.Because of its superior particular performances, it is used and has related to many-sides such as nano electron device, electrochemical material, hydrogen storage material and composite material reinforcement body.
Natural rubber is as a kind of renewable natural resource with superior over-all properties, has snappiness, high strength, high elongation rate and characteristics such as wear-resisting, is widely used in aerospace, defence and military, heavy-duty car, plane tyre, the medical elastomer.Therefore, natural rubber occupies important status in the development of the national economy.Yet,, exist in the non-polar solvent and expand because natural rubber is a non-polar rubber, oil resistant, poor solvent resistance, and because of containing a large amount of unsaturated double-bonds, the chemically reactive height, be easy to crosslinked and oxidation, defectives such as ageing resistance difference, thus limited the range of application of natural rubber.
In order to remedy the defective that natural rubber self exists, the common employing of people adds strengthening agent, vulcanizing agent and various Synergist S-421 95 and prepares native rubber composite material through the mixing method of dry method in the dried glue of natural rubber.But because the mixing process not only consumes energy but also contaminate environment of this method are gone back the serious harm health of operators, and the dispersion effect of packing material in natural rubber that adds is unsatisfactory, causes reinforcing effect undesirable.Therefore, be necessary to provide a kind of preparation to have the method for the native rubber composite material of good over-all properties.
[summary of the invention]
The object of the present invention is to provide a kind of preparation method with native rubber composite material of good over-all properties.
Specifically, the present invention adopts tensio-active agent that carbon nanotube is carried out surface modification and makes its lotus that becomes positively charged, and then with the electronegative direct blend of emulsus natural rubber, utilize the electrostatic absorption principle self-assembly to prepare natural rubber-carbon nano tube composite material (detailed process is as shown in Figure 1).
Specific embodiments of the present invention is as follows:
(1) an amount of carbon nanotube is placed the flask boiling reflux that the vitriol oil and concentrated nitric acid solution are housed, cooling, the deionized water dilution, filtering and washing obtains surface-functionalized carbon nanotube to neutral.
(2) surface-functionalized carbon nanotube that (1) is obtained and an amount of anion surfactant join deionized water for ultrasonic, regulate the pH value, again to wherein adding an amount of cats product, stir the back and remove unnecessary tensio-active agent, obtain carbon nano tube water dispersoid system with deionized water wash.
(3) the carbon nano tube water dispersoid system that (2) is obtained joins in an amount of pre-treatment lactous natural rubber, stirs, and obtains the emulsus natural rubber-carbon nano tube composite material.
(4) with (3) to the emulsus natural rubber-carbon nano tube composite material solidify according to a conventional method, drying obtains the natural rubber-carbon nano tube composite material film.
The deal of the described natural rubber of above embodiment, carbon nanotube, anion surfactant and cats product (in dry weight part, down together) is:
10～50 parts of natural rubbers; 0.2～1.2 part of carbon nanotube;
0.1～0.6 part of anion surfactant; 0.02～0.12 part of cats product.
Carbon nanotube of the present invention, optional multi-walled carbon nano-tubes by the preparation of vapor-phase thermal cracking method, preferred caliber is 10-30nm, pipe range is 5-15 μ m, the multi-walled carbon nano-tubes of purity 〉=95.0%; Described anion surfactant, optional sodium lauryl sulphate, or Sodium dodecylbenzene sulfonate, or sodium polyacrylate, preferably sodium dodecyl sulfate; Described cats product, optional diallyl dimethyl ammoniumchloride, or alkyl glycoside, or cetrimonium bronmide, preferred diallyl dimethyl ammoniumchloride; Described emulsus natural rubber, the optional natural rubber latex that is derived from Brazilian para ruber, or pre-vulcanized natural latex, preferred centrifugal concentrated total solids level are that 60% concentrated natural latex or total solids level are 60% prevulcanized concentrated natural latex.
Therefore, a kind of method of utilizing the static self-assembly to prepare natural rubber-carbon nano tube composite material of the present invention, preferably adopt following embodiment:
(1) be that 10-30nm, pipe range are that the multi-walled carbon nano-tubes of 5-15 μ m, purity 〉=95.0% places the flask boiling reflux 1～2.5 hour that the vitriol oil and concentrated nitric acid solution are housed with the preparation of 0.2～1.2 part of vapor-phase thermal cracking method, caliber, cooling, a large amount of deionized water dilutions, the washing of millipore filtration decompress filter obtains surface-functionalized carbon nanotube to neutral.
(2) the surface-functionalized carbon nanotube that (1) is obtained and 0.1～0.6 part of sodium lauryl sulphate joined deionized water for ultrasonic 0.5 hour, regulate the pH value to 9-11, be 10 diallyl dimethyl ammoniumchloride to wherein adding 0.02～0.12 part of pH value again, after the magnetic agitation 5～7 hours, repeatedly to remove unnecessary tensio-active agent, obtain carbon nano tube water dispersoid system with deionized water wash.
(3) carbon nano tube water dispersoid that (2) obtained system joins that 10～50 parts of pH values are 10, centrifugal concentrated total solids level is 60% concentrated natural latex or total solids level is in 60% the prevulcanized concentrated natural latex, magnetic agitation 20～24 hours obtains the emulsus natural rubber-carbon nano tube composite material.
(4) the emulsus natural rubber-carbon nano tube composite material that (3) are obtained solidifies according to a conventional method, drying obtains the natural rubber-carbon nano tube composite material film.
Carbon nanotube-the native rubber composite material of the present invention's preparation; the homodisperse of carbon nanotube in natural rubber; and it is good with the consistency of natural rubber; for the nano composite material rubber item for preparing excellent combination property provides technical guarantee; and it is simple to have preparation technology; favorable reproducibility, advantage such as accomplish scale production easily.
[description of drawings]
The static self assembling process synoptic diagram of Fig. 1 preparation carbon nanotube-native rubber composite material provided by the invention;
The transmission electron microscope photo of CNT (carbon nano-tube) in natural rubber after the modification of Fig. 2 process the inventive method;
The stereoscan photograph of CNT (carbon nano-tube) in natural rubber after the modification of Fig. 3 process the inventive method.
[embodiment]
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.Except as otherwise noted, the umber that hereinafter adopts is dry weight part.
Embodiment one:
(1) be that 10-30nm, pipe range are that the multi-walled carbon nano-tubes of 5-15 μ m, purity 〉=95.0% places the flask boiling reflux 1.5 hours that the vitriol oil and concentrated nitric acid solution are housed with the preparation of 1 part of vapor-phase thermal cracking method, caliber, cooling, a large amount of deionized water dilutions, the washing of millipore filtration decompress filter obtains surface-functionalized carbon nanotube to neutral.
(2) the surface-functionalized carbon nanotube that (1) is obtained and 0.5 part of sodium lauryl sulphate joined deionized water for ultrasonic 0.5 hour, regulate pH value to 10, be 10 diallyl dimethyl ammoniumchloride to wherein adding 0.1 part of pH again, magnetic agitation after 5 hours with deionized water wash repeatedly to remove unnecessary tensio-active agent, obtain carbon nano tube water dispersoid.
(3) carbon nano tube water dispersoid that (2) are obtained joins that 20 parts of pH values are 10, centrifugal concentrated total solids level is that magnetic agitation 20 hours obtains the emulsus natural rubber-carbon nano tube composite material in 60% the concentrated natural latex.
(4) the emulsus natural rubber-carbon nano tube composite material that (3) are obtained solidifies according to a conventional method, drying obtains the natural rubber-carbon nano tube composite material film.
Embodiment two:
(1) be that 10-30nm, pipe range are that the multi-walled carbon nano-tubes of 5-15 μ m, purity 〉=95.0% places the flask boiling reflux 2 hours that the vitriol oil and concentrated nitric acid solution are housed with the preparation of 0.5 part of vapor-phase thermal cracking method, caliber, cooling, a large amount of deionized water dilutions, the washing of millipore filtration decompress filter obtains surface-functionalized carbon nanotube to neutral.
(2) sodium lauryl sulphate of the surface-functionalized carbon nanotube that (1) is obtained and 0.25 part joined deionized water for ultrasonic 0.5 hour, regulate pH value to 10, be 10 diallyl dimethyl ammoniumchloride to wherein adding 0.05 part of pH value again, magnetic agitation after 6 hours with deionized water wash repeatedly to remove unnecessary tensio-active agent, obtain carbon nano tube water dispersoid.
(3) carbon nano tube water dispersoid that (2) are obtained joins that 40 parts of pH values are 10, centrifugal concentrated total solids level is that magnetic agitation 24 hours obtains the emulsus natural rubber-carbon nano tube composite material in 60% the prevulcanized concentrated natural latex.
(4) the emulsus natural rubber-carbon nano tube composite material that (3) are obtained solidifies according to a conventional method, drying obtains the natural rubber-carbon nano tube composite material film.
Embodiment three:
(1) be that 10-30nm, pipe range are that the multi-walled carbon nano-tubes of 5-15 μ m, purity 〉=95.0% places the flask boiling reflux 1 hour that the vitriol oil and concentrated nitric acid solution are housed with the preparation of 0.8 part of vapor-phase thermal cracking method, caliber, cooling, a large amount of deionized water dilutions, the washing of millipore filtration decompress filter obtains surface-functionalized carbon nanotube to neutral.
(2) the surface-functionalized carbon nanotube that (1) is obtained and 0.4 part of sodium lauryl sulphate joined deionized water for ultrasonic 0.5 hour, regulate pH to 10, be 10 diallyl dimethyl ammoniumchloride to wherein dripping 0.08 part of pH value again, magnetic agitation after 7 hours with deionized water wash repeatedly to remove unnecessary tensio-active agent, obtain carbon nano tube water dispersoid.
(3) carbon nano tube water dispersoid that (2) are obtained joins that 25 parts of pH values are 10, centrifugal concentrated total solids level is that magnetic agitation 22 hours obtains the emulsus natural rubber-carbon nano tube composite material in 60% the prevulcanized concentrated natural latex.
(4) the emulsus natural rubber-carbon nano tube composite material that (3) are obtained solidifies according to a conventional method, drying obtains the natural rubber-carbon nano tube composite material film.
By the microscopic pattern of electron microscopic observation carbon nanotube in natural rubber, as can be seen from Figures 2 and 3, in the prevulcanized concentrated natural latex, present single dispersion through method carbon nano tube modified provided by the invention, combine closely, reached good dispersion effect with latex.
Claims (8)
1, a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material is characterized in that containing following steps, and component wherein is dry weight part:
(1) 0.2～1.2 part of carbon nanotube is placed the flask boiling reflux that the vitriol oil and concentrated nitric acid solution are housed, cooling, the deionized water dilution, filtering and washing obtains surface-functionalized carbon nanotube to neutral.
(2) the surface-functionalized carbon nanotube that (1) is obtained and 0.1～0.6 portion of anion surfactant join deionized water for ultrasonic, regulate the pH value, again to wherein dripping 0.02～0.12 part of cats product, remove unnecessary tensio-active agent with deionized water wash after stirring, obtain carbon nano tube water dispersoid system.
(3) the carbon nano tube water dispersoid system that (2) is obtained is added drop-wise in 10～50 parts of emulsus natural rubbers, stirs, and obtains the emulsus natural rubber-carbon nano tube composite material.
(4) with (3) to the emulsus natural rubber-carbon nano tube composite material solidify according to a conventional method, drying obtains the natural rubber-carbon nano tube composite material film.
2,, it is characterized in that described carbon nanotube is is that 10-30nm, pipe range are the multi-walled carbon nano-tubes of 5-15 μ m, purity 〉=95.0% by vapor-phase thermal cracking method preparation, caliber according to the described a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material of claim 1.
3, according to the described a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material of claim 1, it is characterized in that described anion surfactant is selected from sodium lauryl sulphate, Sodium dodecylbenzene sulfonate and sodium polyacrylate.
4,, it is characterized in that anion surfactant is a sodium lauryl sulphate according to the described a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material of claim 3.
5, according to the described a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material of claim 1, it is characterized in that described cats product is selected from diallyl dimethyl ammoniumchloride, alkyl glycoside and cetrimonium bronmide.
6,, it is characterized in that cats product is a diallyl dimethyl ammoniumchloride according to the described a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material of claim 5.
7, a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material according to claim 1 is characterized in that it is that 60% concentrated natural latex and total solids level are 60% prevulcanized concentrated natural latex that described emulsus natural rubber is selected from the natural rubber latex of Brazilian para ruber, pre-vulcanized natural latex, centrifugal concentrated total solids level.
8,, it is characterized in that the emulsus natural rubber is that centrifugal concentrated total solids level is that 60% concentrated natural latex and total solids level are 60% prevulcanized concentrated natural latex according to the described a kind of method of utilizing the static self-assembly to prepare carbon nanotube-native rubber composite material of claim 7.
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