CN1706772A - Prepn process of composite material of metal or metal oxide and carbon nanotube - Google Patents
Prepn process of composite material of metal or metal oxide and carbon nanotube Download PDFInfo
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- CN1706772A CN1706772A CN 200410046388 CN200410046388A CN1706772A CN 1706772 A CN1706772 A CN 1706772A CN 200410046388 CN200410046388 CN 200410046388 CN 200410046388 A CN200410046388 A CN 200410046388A CN 1706772 A CN1706772 A CN 1706772A
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- ionic liquid
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- tetramethyl guanidine
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Abstract
The present invention is preparation process of composite material of metal or metal oxide and carbon nanotube inside ionic liquid through microwave heating. Specifically, inside room temperature ionic liquid as medium of tetramethyl guanidine trifluoromethanesulfonate, tetramethyl guanidine trifluoroacetate, tetramethyl guanidine lactate, tetramethyl guanidine formate, tetramethyl guanidine perchlorate, etc, chloroauric acid, chloroplatinic acid, ruthenium chloride, palladium chloride, metal nitrate and other metal compound easy to take heat chemical reaction is dissolved, and carbon nanotube is ultrasonically dispersed to form stable dispersant system. The system is microwave heated for some period to obtain the composite material of metal or metal oxide and carbon nanotube. The said process is fast and simple, and has easy separation between the product and the ionic liquid and reuse of the ionic liquid.
Description
Technical field
The present invention relates to a kind of method of utilizing ionic liquid and microwave heating technique to prepare metal or metal oxide/carbon nano-tube composite material.
Background technology
Because carbon nanotube (CNTs) has performances such as unique electricity, calorifics, mechanics, magnetics, fields such as emission on the scene, molecular electronic device, composite reinforcing material, hydrogen storage material, catalysis have wide practical use.Therefore since coming out, obtained people's attention always.Increasingly mature along with the carbon nanotube synthetic technology, the low-cost carbon nanotube of producing in enormous quantities is achieved success, and explores and the purposes of exploitation carbon nanotube becomes the hot issue that people pay close attention to.The carbon nano tube compound material that with the carbon nanotube is matrix gives carbon nanotube new characteristic, for the application of carbon nanotube provides new approach.Metal refining or metal oxide on carbon nanotube make carbon nano tube compound material useful as catalysts, functional materials etc., have important application value.
Ionic liquid at room temperature is a melting salt, by negatively charged ion and cation composition.Ionic liquid commonly used is non-volatile, can not pollute, thereby be described as green solvent.Many ionic liquids have very wide liquid temperature scope.Ionic liquid is an excellent solvent, and solubilized polarity and nonpolar organism, inorganics have and be easy to and other separating substances, advantage such as can recycle.In recent years, ion liquid research causes extensive concern.
The chemical reaction of microwave heating is a kind of new Green Chemistry method, is applied at inorganic synthetic, aspects such as environmental chemistry, especially organic synthesis.Microwave heating technique and ionic liquid bonded chemical reaction are applied, and the research of especially using in organic synthesis is maximum, and the application aspect the inorganic chemistry reaction also seldom.Ionic liquid is combined with microwave heating, chemical reaction velocity is increased substantially, the selectivity of reaction and transformation efficiency obtain improvement in various degree, are very promising technology therefore.
Summary of the invention
The object of the present invention is to provide a kind of with ionic liquid and microwave heating technique combination, utilize ionic liquid to be medium, with microwave heating as type of heating, make metallic compound that thermal chemical reaction take place under certain condition, generate metal or metal oxide nano-material, be deposited on the CNTs, thereby make the method for metal or metal oxide/CNT matrix material.
The invention provides a kind of method for preparing metal or burning/carbon mano-tube composite.This method is for the first time with ionic liquid and microwave heating technique combination, metal refining and metal oxide on CNTs.Ionic liquid is eco-friendly green solvent, utilizes microwave heating, can make ionic liquid reach higher temperature in a short period of time, and being reflected in the very short time in the ionic liquid medium finished.Ionic liquid can recycle, and product is not produced and pollutes.In actual production process, can reduce technical process, thereby reduce cost.Therefore the present invention has important practical value.
Ionic liquid of the present invention is the ionic liquid that tetramethyl guanidine positively charged ion and different anions (comprising acid radical anions such as trifluoromethane sulfonic acid negatively charged ion, trifluoroacetic acid negatively charged ion, lactic acid negatively charged ion, formic acid negatively charged ion, perchloric acid negatively charged ion, acrylic anionic, methacrylic acid anion) are formed, they and CNTs have good affinity, CNTs is evenly dispersed in wherein, and multiple metal-salt is had good dissolving ability.
Metallic compound of the present invention comprises that the metallic compound of thermal chemical reaction easily takes place for hydrochloro-auric acid, Platinic chloride, ruthenium chloride, Palladous chloride, rhodium chloride, tindichloride, metal nitrate, metal acetate etc.They can be dissolved in the ionic liquid.
That CTNs of the present invention comprises is single, double, many walls CNTs and carry out the above-mentioned CNTs of surface modification.
The method that the present invention prepares metal or metal oxide/CNT is as follows: ionic liquid is contained in the glass reactor, a certain amount of metallic compound is dissolved in wherein, add a certain amount of CNTs then, the ultrasonic CNTs of making is evenly dispersed in the ionic liquid solution.Reactor is put into microwave heating installation, and under certain power, the reactant in the irradiation reactor behind the reaction certain hour, stops microwave heating, and termination reaction obtains metal or metal oxide/CNT matrix material.
The present invention has following characteristics:
1. the present invention combines ionic liquid and microwave heating, is a green technology.
2. chemical reaction involved in the present invention, speed of response is fast, and reaction generally can be finished in ten minutes.
3. product yield height.
4. to adopt ionic liquid be solvent in the present invention, can easily realize separating of product and solvent, and ionic liquid can be recycled.
Embodiment
Embodiment 1
Measure 3 milliliters of ionic liquid trifluoromethane sulfonic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of Platinic chlorides, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 120W, heated 3 minutes, the platinum of the Pt nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 2
Measure 3 milliliters of ionic liquid trifluoromethane sulfonic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of hydrochloro-auric acids, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the gold of the gold nano grain/CNT matrix material that obtained surface deposition.
Embodiment 3
Measure 3 milliliters of ionic liquid trifluoromethane sulfonic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of ruthenium chlorides, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the ruthenium of the ruthenium nano-particle/CNT matrix material that obtained surface deposition.
Embodiment 4
Measure 3 milliliters of ionic liquid trifluoromethane sulfonic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 20 milligrams of europium nitrates, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the europium sesquioxide of the europium sesquioxide nano particle/CNT matrix material that obtained surface deposition.
Embodiment 5
Measure 3 milliliters of ionic liquid trifluoromethane sulfonic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 20 milligrams of zinc acetates, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the zinc oxide of the Zinc oxide nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 6
Measure 3 milliliters of ionic liquid trifluoroacetic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 20 milligrams of europium nitrates, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the europium sesquioxide of the europium sesquioxide nano particle/CNT matrix material that obtained surface deposition.
Embodiment 7
Measure 3 milliliters of ionic liquid trifluoroacetic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 20 milligrams of zinc acetates, dissolve in ionic liquid.Add the CNTs15 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the zinc oxide of the Zinc oxide nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 8
Measure 3 milliliters of ionic liquid trifluoroacetic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of Platinic chlorides, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 120W, heated 3 minutes, the platinum of the Pt nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 9
Measure 3 milliliters of ionic liquid lactic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of hydrochloro-auric acids, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the gold of the gold nano grain/CNT matrix material that obtained surface deposition.
Embodiment 10
Measure 3 milliliters of ionic liquid lactic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of ruthenium chlorides, dissolve in ionic liquid.Add the CNTs20 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 120W, heated 3 minutes, the ruthenium of the ruthenium nano-particle/CNT matrix material that obtained surface deposition.
Embodiment 11
Measure 3 milliliters of ionic liquid lactic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of Platinic chlorides, dissolve in ionic liquid.Add the CNTs15 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 120W, heated 3 minutes, the platinum of the Pt nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 12
Measure 3 milliliters of ionic liquid formic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of hydrochloro-auric acids, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the gold of the gold nano grain/CNT matrix material that obtained surface deposition.
Embodiment 13
Measure 3 milliliters of ionic liquid formic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of ruthenium chlorides, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the ruthenium of the ruthenium nano-particle/CNT matrix material that obtained surface deposition.
Embodiment 14
Measure 3 milliliters of ionic liquid formic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 20 milligrams of europium nitrates, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the europium sesquioxide of the europium sesquioxide nano particle/CNT matrix material that obtained surface deposition.
Embodiment 15
Measure 3 milliliters of ionic liquid perchloric acid tetramethyl guanidines, place 10 milliliters glass reactor, add 20 milligrams of zinc acetates, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the zinc oxide of the Zinc oxide nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 16
Measure 3 milliliters of ionic liquid perchloric acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of hydrochloro-auric acids, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the gold of the gold nano grain/CNT matrix material that obtained surface deposition.
Embodiment 17
Measure 3 milliliters of ionic liquid vinylformic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of Platinic chlorides, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the platinum of the Pt nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 18
Measure 3 milliliters of ionic liquid vinylformic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of hydrochloro-auric acids, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the gold of the gold nano grain/CNT matrix material that obtained surface deposition.
Embodiment 19
Measure 3 milliliters of ionic liquid methacrylic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of Platinic chlorides, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the platinum of the Pt nanoparticle/CNT matrix material that obtained surface deposition.
Embodiment 20
Measure 3 milliliters of ionic liquid methacrylic acid tetramethyl guanidines, place 10 milliliters glass reactor, add 10 milligrams of hydrochloro-auric acids, dissolve in ionic liquid.Add the CNTs10 milligram again, ultra-sonic dispersion CNTs is evenly dispersed in the ionic liquid it, forms steady suspension.Glass reactor is put into microwave heating installation, under the power condition of 80W, heated 1 minute, the gold of the gold nano grain/CNT matrix material that obtained surface deposition.
Claims (5)
1. method for preparing metal or metal oxide/carbon nano-tube composite material, key step is:
The metallic compound that adds the 1-20 milligram in every milliliter of ionic liquid, the ratio that adds the 1-10 milligram in every milliliter of ionic liquid is dispersed in carbon nanotube and forms dispersion system in the ionic liquid again, 80-120W microwave heating 1-5 minute obtains metal or metal oxide/carbon nano-tube composite material;
Wherein metallic compound is the metallic compound that thermal chemical reaction easily takes place;
Wherein ionic liquid for can the dissolution of metals compound and the stable dispersion carbon nanotube, positively charged ion is the ionic liquid of tetramethyl guanidine.
2. the method for claim 1 is characterized in that, used metallic compound is that hydrochloro-auric acid, Platinic chloride, ruthenium chloride, tindichloride, Palladous chloride, rhodium chloride, metal nitrate or metal acetate can be dissolved in the metallic compound in the ionic liquid.
3. the method for claim 1, it is characterized in that used ionic liquid is the ionic liquid of trifluoromethane sulfonic acid tetramethyl guanidine, trifluoroacetic acid tetramethyl guanidine, lactic acid tetramethyl guanidine, formic acid tetramethyl guanidine, perchloric acid tetramethyl guanidine, vinylformic acid tetramethyl guanidine or methacrylic acid tetramethyl guanidine energy dissolution of metals compound and stable dispersion carbon nanotube.
4. the method in the claim 1 is characterized in that, used carbon nanotube is single, double, many walls and the carbon nanotube that carries out surface modification.
5. the method for claim 1 is characterized in that, carbon nanotube is to use ultra-sonic dispersion in ionic liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100463885A CN1312032C (en) | 2004-06-08 | 2004-06-08 | Prepn process of composite material of metal or metal oxide and carbon nanotube |
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| CNB2004100463885A CN1312032C (en) | 2004-06-08 | 2004-06-08 | Prepn process of composite material of metal or metal oxide and carbon nanotube |
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| CN1706772A true CN1706772A (en) | 2005-12-14 |
| CN1312032C CN1312032C (en) | 2007-04-25 |
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| CN100366647C (en) * | 2006-05-19 | 2008-02-06 | 浙江大学 | Anion type polymer containing tetramethylguanidine cation and its preparation method and uses |
| CN100366651C (en) * | 2006-05-19 | 2008-02-06 | 浙江大学 | Cross-linked anion polymer containing tetramethylguanidine cation and its preparation method and uses |
| CN101029147B (en) * | 2007-03-05 | 2010-05-19 | 四川大学 | Metal compound/carbon nano-composite material and its production |
| CN101559938B (en) * | 2008-04-18 | 2011-05-11 | 中国科学院大连化学物理研究所 | Preparation method of high-graphitized nanometer carbon material |
| ES2359819A1 (en) * | 2009-11-13 | 2011-05-27 | Universidad De Vigo | E-caprolactama obtaining procedure from the october of cyclohexanona. (Machine-translation by Google Translate, not legally binding) |
| CN101787502B (en) * | 2010-01-19 | 2011-10-05 | 中国科学院化学研究所 | Method for preparing metal, metallic oxide or metallic hydroxide and carbon nano tube composite |
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| CN100366647C (en) * | 2006-05-19 | 2008-02-06 | 浙江大学 | Anion type polymer containing tetramethylguanidine cation and its preparation method and uses |
| CN100366651C (en) * | 2006-05-19 | 2008-02-06 | 浙江大学 | Cross-linked anion polymer containing tetramethylguanidine cation and its preparation method and uses |
| CN101029147B (en) * | 2007-03-05 | 2010-05-19 | 四川大学 | Metal compound/carbon nano-composite material and its production |
| CN101559938B (en) * | 2008-04-18 | 2011-05-11 | 中国科学院大连化学物理研究所 | Preparation method of high-graphitized nanometer carbon material |
| CN101780949B (en) * | 2009-01-19 | 2011-12-07 | 中国科学院化学研究所 | Method for preparing multi-walled carbon nano-tube |
| CN102040212B (en) * | 2009-10-23 | 2013-01-09 | 清华大学 | Carbon nano tube composite structure |
| ES2359819A1 (en) * | 2009-11-13 | 2011-05-27 | Universidad De Vigo | E-caprolactama obtaining procedure from the october of cyclohexanona. (Machine-translation by Google Translate, not legally binding) |
| CN101787502B (en) * | 2010-01-19 | 2011-10-05 | 中国科学院化学研究所 | Method for preparing metal, metallic oxide or metallic hydroxide and carbon nano tube composite |
| CN102324302A (en) * | 2011-06-13 | 2012-01-18 | 郑州大学 | Preparation method of super capacitor based on one-dimensional metal-carbon nano tube coaxial heterojunction |
| CN102324302B (en) * | 2011-06-13 | 2012-11-07 | 郑州大学 | Preparation method of super capacitor based on one-dimensional metal-carbon nano tube coaxial heterojunction |
| CN103594710A (en) * | 2012-08-13 | 2014-02-19 | 清华大学 | Preparation method for negative electrode of lithium ion battery |
| CN103594681A (en) * | 2012-08-13 | 2014-02-19 | 清华大学 | Preparation method for negative electrode of lithium ion battery |
| CN103594681B (en) * | 2012-08-13 | 2016-06-08 | 清华大学 | The preparation method of lithium ion battery negative |
| CN104297310A (en) * | 2014-11-01 | 2015-01-21 | 吴玲 | Preparation and using method for glucose ampere detector based on novel nanocomposite material |
| CN107774247A (en) * | 2017-10-25 | 2018-03-09 | 吉林大学 | A kind of carbon dioxide electrochemical reduction catalyst and preparation method thereof |
| CN107774247B (en) * | 2017-10-25 | 2020-06-05 | 吉林大学 | Carbon dioxide electrochemical reduction catalyst and preparation method thereof |
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| CN112121862A (en) * | 2020-10-15 | 2020-12-25 | 江西赣江新区有机硅创新研究院有限公司 | Magnetic immobilized platinum catalyst and preparation method and application thereof |
| CN115785514A (en) * | 2022-11-23 | 2023-03-14 | 苏州大学 | Zinc oxide coated modified hollow thermal expansion microsphere and preparation method and application thereof |
| CN115785514B (en) * | 2022-11-23 | 2023-08-11 | 苏州大学 | Zinc oxide coated modified hollow thermal expansion microsphere and preparation method and application thereof |
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