CN103044914A - Modified CNT (carbon nano tube)/ nylon composite material - Google Patents
Modified CNT (carbon nano tube)/ nylon composite material Download PDFInfo
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- CN103044914A CN103044914A CN 201210594361 CN201210594361A CN103044914A CN 103044914 A CN103044914 A CN 103044914A CN 201210594361 CN201210594361 CN 201210594361 CN 201210594361 A CN201210594361 A CN 201210594361A CN 103044914 A CN103044914 A CN 103044914A
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Abstract
The invention provides a modified CNT/ nylon composite material. The composite comprises components as follows: a multi-walled CNT, ethanediamine, thionyl chloride, concentrated nitric acids, concentrated sulfuric acids, tetrahydrofuran, distilled water, absolute ethyl alcohol and nylon 1212. The invention further provides a composite method for the modified CNT and a manufacturing technique for the modified CNT/ nylon composite material to obtain the CNT/ nylon composite material with excellent performance.
Description
Technical field
The present invention relates to chemical field, particularly a kind of modified carbon nano-tube/nylon composite materials.
Background technology
The ideal that carbon nanotube is considered to matrix material strengthens body, can improve the toughness of matrix material, and intensity and electroconductibility etc. have great researching value.But, because specific surface area and the surface energy of carbon nanotube are larger, so that carbon nanotube is easy to reunite, affected the dispersion of carbon nanotube in matrix.And carbon nano tube surface is smooth, is nonpolar, is insoluble to general organic solvent, all incompatible with all polymkeric substance, so that the interface interaction of matrix material is not strong, therefore, needs are first with carbon nano-tube modification, and are compound with polymkeric substance again, can obtain a kind of matrix material of excellent performance.
Summary of the invention
The present invention proposes a kind of modified carbon nano-tube/nylon composite materials, has solved the dispersion of carbon nanotube in polymkeric substance and the interface binding power problem of carbon nanotube and polymeric matrix in the prior art, obtains a kind of matrix material of mechanical property excellence.
Technical scheme of the present invention is achieved in that modified carbon nano-tube, multi-walled carbon nano-tubes, quadrol, sulfur oxychloride, concentrated nitric acid, the vitriol oil, tetrahydrofuran (THF), distilled water, dehydrated alcohol, nylon 1212.
The invention has the beneficial effects as follows:
(1) the present invention has obtained a kind of modified carbon nano-tube, solved the dispersion of carbon nanotube in polymkeric substance and with the interface binding power problem of polymeric matrix.
(2) the present invention has obtained a kind of modified carbon nano-tube/nylon composite materials of mechanical property excellence.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, the below will do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art, apparently, accompanying drawing in the following describes only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the production technological process of modified carbon nano-tube/nylon 1212 of the present invention.
Embodiment
The present invention is through extensive and deep research, and is compound by the multi-walled carbon nano-tubes of quadrol modification and nylon 1212 by adopting, and produces a kind of matrix material of modified carbon nano-tube/nylon 1212, thereby finishes the present invention.Fig. 1 is the production technological process of modified carbon nano-tube/nylon 1212 of the present invention, step 10: the nitration mixture (vitriol oil: concentrated nitric acid=3: 1) multi-walled carbon nano-tubes is carried out the acid cutting; Step 20: sour cutting carbon nanotubes and sulfur oxychloride reaction make the carboxyl of carbon nano tube surface be converted into acyl chlorides; Step 30: get quantitative quadrol and carbon pipe, 2: 1 ratio is carried out graft reaction to the carbon pipe; Step 40: behind the graft reaction, obtain modified carbon nano-tube; Step 50: modified carbon nano-tube and nylon 1212 be melt blending on the Brabender rheometer; Step 60: after a blend part shreds drying, be extruded into silk at XNR-400A type Melt Flow Rate Measurer, in extrusion, limit traction nylon 1212 matrix material obtains modified carbon nano-tube/nylon 1212 matrix material
Multi-walled carbon nano-tubes
The unique texture of carbon nanotube has determined that it has many special physics and chemistry character.The C=C covalent linkage that forms carbon nanotube is the most stable chemical bond of nature, so that carbon nanotube has very excellent mechanical property.The mechanical property of carbon nanotube and little diameter thereof and large length-to-diameter ratio will be brought better reinforced effects to carbon nano tube compound material.
The multi-walled carbon nano-tubes that the present invention uses has adopted the CVD method to produce.
Preferably, described multi-walled carbon nano-tubes mean diameter is less than 8nm, length 10～30m, and purity is greater than 95% (by rare nitric acid purifying).
Modified carbon nano-tube
Take by weighing the original multi-walled carbon nano-tubes of 5g (p-MWNTs), place the nitration mixture (vitriol oil: concentrated nitric acid=3: 1) 50 ℃ of backflow 4h of 300ml, then vacuum filtration, the black solid that obtains is filtered with distilled water flushing repeatedly, until filtrate pH value near neutrality till, obtain sour cutting carbon nanotubes (a-MWNTs), the product that obtains is placed 80 ℃ of dry 24h of vacuum drying oven, obtain the modified carbon nano-tube after acid is cut; Carbon nanotube after the acid cutting and sulfur oxychloride are reacted backflow 24h, the carboxyl of carbon nano tube surface is converted to acyl chlorides.After washing the dechlorination sulfoxide with tetrahydrofuran (THF) afterwards, vacuum-drying 24h under room temperature.Measure an amount of quadrol and carbon pipe, behind 130-140 ℃ of back flow reaction 24h, be cooled to room temperature in 2: 1 ratios.It is dry that reaction product is leached the rear washing with alcohol of using, and obtains the function modified carbon nanotube of quadrol (MWNTs-EDA).
Nylon 1212
Tynex is commonly called as nylon (Nylon), English name Polyamide (being called for short PA), density 1.15g/cm3; , be contain on the molecular backbone chain recurring amide radical group-[NHCO]-the thermoplastic resin general name.PA has good over-all properties, comprise mechanical property, thermotolerance, wearability, chemical proofing and self lubricity, and frictional coefficient is low, certain flame retardant resistance is arranged, be easy to processing, be suitable for improving performance and broadened application scope with glass fibre and other filler filling enhancing modified.
Other components: sulfur oxychloride, concentrated nitric acid, the vitriol oil, tetrahydrofuran (THF), distilled water, dehydrated alcohol is marketable material.
Below in conjunction with specific embodiment, further set forth the present invention.The experimental technique of unreceipted actual conditions in the following example is measured according to national standard usually.If there is not corresponding national standard, then carry out according to general international standard, normal condition or according to the condition that manufacturer advises.Unless otherwise indicated, otherwise all umbers are weight part, and all per-cents are weight percentage, and described polymericular weight is number-average molecular weight.
Unless otherwise defined or explanation, same meanings of being familiar with of all specialties used herein and scientific words and those skilled in the art.Any method similar or impartial to described content and material all can be applicable in the inventive method in addition.
The recombination process of modified carbon nano-tube and nylon 1212 is as follows:
With modified carbon nano-tube, original carbon nanotube and nylon 1212 melt blending on the Brabender rheometer.The melt blending condition:
Blending temperature: 210 ℃ are carried out melt blending;
Screw speed is: 30 turn/min;
The melt blending time: 10min.
After a blend part that obtains shredded drying, be extruded into silk at XNR-400A type Melt Flow Rate Measurer, in extrusion, limit traction nylon 1212 matrix material obtains matrix material behind the heat-traction, and draw ratio can be tried to achieve by cross-sectional area; Another part by compression molding, is cut out to get standard test specimen, and test tensile strength and elongation at break, draw speed are 50mm/min.Simultaneously, by restrained stretching length, obtain normal temperature traction sample, draw ratio can be tried to achieve by cross-section variation.
Found through experiments, original carbon nanotube and nylon 1212 matrix material are when melt blending, increase along with content of carbon nanotubes, the moment of torsion of system begins rapid increase, change after 0.5 part less, and modified carbon nano-tube, because carbon nanotube contains the amino group identical with nylon, so that the consistency of the carbon nanotube after the modification and nylon is greatly improved, the moment of torsion of system is not along with the increase of content of carbon nanotubes changes substantially, and the dispersing property of carbon nanotube and nylon must be mentioned.
By mechanics property analysis, although amination treatment can be improved the consistency between carbon nanotube and the nylon 1212, the degree of improving is limited, therefore along with the raising of content of carbon nanotubes, the reunion degree increases, and the uncompatibility at interface increases, so the intensity of material descends again thereupon; And elongation at break descends gradually, and the adding of carbon nanotube is described, stoichiometric is not how much, all is the consistency that can reduce composite system.For original carbon nanotube, the tensile strength of finding matrix material is not very stable, when add-on is less, impact is not very large on tensile strength, when add-on increases, tensile strength and elongation at break descend more obvious, mainly are that original carbon nanotube and nylon 1212 matrix phase capacitive are bad, cause overall performance to descend.Simultaneously also explanation, modified carbon nano-tube could be significantly improved to the mechanical property of matrix material.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a modified carbon nano-tube/nylon composite materials is characterized in that, described composition component comprises following component: modified carbon nano-tube, quadrol, sulfur oxychloride, concentrated nitric acid, the vitriol oil, tetrahydrofuran (THF), distilled water, dehydrated alcohol, nylon 1212.
2. modified carbon nano-tube/nylon composite materials according to claim 1 is characterized in that, the nylon 1212 fusing point: 170 ℃-176 ℃; Size-grade distribution: 80-250 order.
3. modified carbon nano-tube/nylon composite materials according to claim 1 is characterized in that, modified carbon nano-tube comprises: contain following component: multi-walled carbon nano-tubes, quadrol, sulfur oxychloride, concentrated nitric acid, the vitriol oil, tetrahydrofuran (THF), distilled water, dehydrated alcohol.
4. modified carbon nano-tube/nylon composite materials according to claim 3 is characterized in that, modified carbon nano-tube is through multi-walled carbon nano-tubes and quadrol grafting and be modified.
5. modified carbon nano-tube/nylon composite materials according to claim 3 is characterized in that, caliber: 10-30nm, purity＞90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210594361 CN103044914A (en) | 2012-12-10 | 2012-12-10 | Modified CNT (carbon nano tube)/ nylon composite material |
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| CN 201210594361 CN103044914A (en) | 2012-12-10 | 2012-12-10 | Modified CNT (carbon nano tube)/ nylon composite material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107227018A (en) * | 2017-05-27 | 2017-10-03 | 清远初曲智能科技有限公司 | A kind of carbon nano-tube modification nylon fire proofing and preparation method thereof |
| CN115595725A (en) * | 2022-12-14 | 2023-01-13 | 石家庄海飞音机电设备有限公司（Cn） | Flame-retardant filter cotton and preparation method thereof |
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2012
- 2012-12-10 CN CN 201210594361 patent/CN103044914A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107227018A (en) * | 2017-05-27 | 2017-10-03 | 清远初曲智能科技有限公司 | A kind of carbon nano-tube modification nylon fire proofing and preparation method thereof |
| CN107227018B (en) * | 2017-05-27 | 2018-05-11 | 清远初曲智能科技有限公司 | A kind of carbon nano-tube modification nylon fire proofing and preparation method thereof |
| CN115595725A (en) * | 2022-12-14 | 2023-01-13 | 石家庄海飞音机电设备有限公司（Cn） | Flame-retardant filter cotton and preparation method thereof |
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Application publication date: 20130417 |