CN102924751A - Preparation method for nanocarbon fluid - Google Patents

Preparation method for nanocarbon fluid Download PDF

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Publication number
CN102924751A
CN102924751A CN2012104807222A CN201210480722A CN102924751A CN 102924751 A CN102924751 A CN 102924751A CN 2012104807222 A CN2012104807222 A CN 2012104807222A CN 201210480722 A CN201210480722 A CN 201210480722A CN 102924751 A CN102924751 A CN 102924751A
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nano
carbon
polyetheramine
carbon material
carbonoxide
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王雁冰
陈娜
李文静
周晨光
彭睿
魏冲
程龙山
黄志雄
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a preparation method for a novel nanocarbon fluid. The method comprises the following steps: adding the original nanocarbon material into strongly acidic oxidation liquid (the volume ratio of concentrated sulfuric acid to concentrated nitric acid is 3:1) to obtain an active carbon oxide material with the surface containing -COOH; adding amino-containing polyether amine serving as a modifier into the suspension liquid of the active carbon oxide material under the conditions of ultrasonic and magnetic stirring, performing acid-base reaction on the amino and carboxyl on the interface of the polyether amine and the carbon oxide material and grafting the polyether amine and the carbon oxide; and adjusting the type and the using amount of the polyether amine to obtain the nanocarbon fluid. The method is simple, effectively controls and increases the grafting ratio of the polyether amine on the surface of the nanocarbon material and is applicable to synthesis of various carbon material fluids. The nanocarbon fluid material prepared by the method has hydrophilicity, lipophilicity and good application prospect in aspects of coating, plastic, rubber, functional materials and the like.

Description

A kind of preparation method of nano-sized carbon fluid
Technical field
The present invention relates to carbon modified material function Material Field, particularly a kind of preparation method of novel nano carbon fluid.
Background technology
Nano-carbon material is of a great variety, mainly contains the nano-carbon materials such as nanometer carbon black, nano-graphite, Nano diamond, Graphene, carbon nanotube or carbon nano fiber.Wherein, nanometer carbon black mainly is used as the tinting material of strengthening agent, printing ink, coating and the plastics of rubber as a kind of ancient Industrial products.Along with the development of novel nano carbon material and polymer matrix composite, nano-carbon material is widely used as the strongthener of polymer matrix composite, but the mechanical property of this matrix material of Effective Raise and electrical property.But the nano-carbon material particle diameter is little, and specific surface area is large, is very easy to reunite.When the preparation nano-carbon material strengthens polymer matrix composite, the nano-carbon material of reuniting can not be dispersed in the polymeric matrix effectively, cause nano-carbon material after the moulding to strengthen polymer matrix composite and hole occurs, the problems such as interface starved have a strong impact on the use properties that nano-carbon material strengthens polymer matrix composite.In addition, the structure that the nano-carbon material particle is loose porous is so that nano-carbon material has powerful chemical adsorptivity, in the storage process of nano-carbon material, nano-carbon material can absorb the materials such as airborne moisture, and these materials are the reunion of aggravation nano-carbon material further.
For further widening the range of application of nano-carbon material, the functional nano carbon material of synthesizing new, investigation of materials persons have proposed the novel method of a lot of nano-carbon material modifications.
Find through the literature search to existing nano-carbon material modification, modified method mainly comprises the following aspects:
1. nano-carbon material is not carried out surface activation process, directly at polymer organism such as nano-carbon material surface grafting polyoxyethylene glycol, 7-sulfydryl propyl trimethoxy silicanes.Carbon material surface exists the inertia groups such as carbonyl, is difficult to and macromolecule organic generation chemical reaction.The carbon modified material surface macromolecule organic grafting amount that this method of modifying obtains is very low, and modified effect is very little.
2. nano-carbon material is carried out surface activation process, then at activated carbon material surface grafting macromolecule organic.But the activating group preparation process is complicated, and nano-carbon material modification rear surface activating group content is less.Although the method has been improved original nano-carbon material reactionlessness to a great extent, to the DeGrain that improves of nano-carbon material reunion.
3. nano-carbon material is carried out surface activation process, then at activated carbon material surface second grafting polymer organism.The method is at a kind of organopolysiloxane that quaternary ammonium group is arranged of carbonoxide material surface grafting, and then grafted polyethylene ethylene glycol, obtains macromolecule modified nano-carbon material particle.This carbon material particle sharply increases through secondary grafting surface organic matter content, so that carbon modified material particle becomes fluid state by graininess.But this method of modifying reaction process is complicated, and can not effectively control the carrying out of reaction.
4. at supercritical CO 2Middle preparation small molecules grafting carbon material has obtained a kind of nano-carbon material particle of favorable dispersity.This method of modifying requires high to experimental installation, high to the purity requirement of carbon material and small-molecule substance, the impurity of a little can cause the free radical inactivation, and the grafting process is produced inhibition.
The present invention adopts the means such as grafting process of oxidation nanometer carbon material, acid-base reaction principle control polyetheramine and carbon material, has obtained a kind of highly active nano oxidized carbon material, and then graft polyether amine, has obtained a kind of novel nano carbon fluid.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method that a kind of simple, controlled nano-sized carbon fluid is provided, the nano-sized carbon fluid of the method preparation is a kind of amphipathic functional materials, can be dispersed in well in coating, plastics, rubber and the functional polymer matrix.
The present invention solves its technical problem and adopts following technical scheme:
The preparation method of nano-sized carbon fluid provided by the invention, specifically: first original nano-carbon material is joined in the strongly-acid oxidation solution, the strongly-acid oxidation solution is V (dense H 2SO 4): V (dense HNO 3)=3:1, obtaining a kind of surface contains-the active oxidation carbon material of COOH; Then under the condition of ultrasonic and magnetic agitation, take the polyetheramine that contains amido as properties-correcting agent, join in the active oxidation carbon material suspension, amido and carboxyl are finished the grafting of polyetheramine and carbonoxide material in polyetheramine and carbonoxide material interface generation acid-base reaction; By regulating type and the consumption of polyetheramine, can obtain being under the room temperature polyethex amine modification carbon material particle of flow-like.
The preparation method of described nano-sized carbon fluid, its step comprises:
(1) carbonoxide material:
The vitriol oil, concentrated nitric acid are configured to the strongly-acid oxidation solution by proportioning, join in the Erlenmeyer flask that fills original carbon material, obtain carbonoxide material mixing liquid; Mixed solution is ultrasonic complete to the carbon material oxidation, obtain carbonoxide material reaction solution; With carbonoxide material reaction solution dialyse, drying and processing, obtain carbonoxide material particle, for subsequent use;
(2) acid functional mass contg assessment:
Configure rare HCl, dilute NaOH solution, utilize acid base titration principle assessment acidic functionality-COOH at the grafting content of carbon material surface;
(3) carbonoxide material/polyetheramine graft reaction:
Get an amount of carbonoxide material, be dispersed in the deionized water, obtain the carbonoxide material suspension; Determined the consumption of polyetheramine by the acid-base reaction principle, this polyetheramine is dissolved in the deionized water, obtain polyether amine solution; The carbon material hanging drop is fixed in the polyether amine solution, and ultrasonic agitation to carbonoxide material and polyetheramine reacts completely, and obtains carbonoxide material/polyetheramine reaction solution;
(4) oven dry carbonoxide material/polyetheramine reaction solution;
Through above-mentioned steps, obtain described nano-sized carbon fluid.
Described original nano-carbon material can adopt nanometer carbon black, nano-graphite, Nano diamond, Graphene, carbon nanotube or carbon nano fiber.
Described polyetheramine can adopt polyether monoamine, polyether diamine, polyethers triamine, polytetramethylene diethyl alcohol radical polyetheramine or aliphatic amine polyoxyethylene ether.
Dense H described in the above-mentioned steps (1) 2SO 4Mass concentration be 98%, described dense HNO 3Mass concentration be 68%.
The concentration of rare HCl described in the above-mentioned steps (2) and rare NaOH is 0.01 mol/L.
The present invention has following advantage and benefit compared with the prior art:
1. nano-carbon material is carried out acidification, Effective Raise carbon material surface-COOH content.Be conducive to polyetheramine and nano-carbon material surface-COOH graft reaction occurs, greatly improved the percentage of grafting of polyetheramine on the nano-carbon material surface.
2. the dispersion technology such as ultrasonic, magnetic agitation have been used, effectively improve nano-carbon material particle, the polyetheramine dispersion state in solvent, for-COOH and polyetheramine surface group provide good reaction environment, further increase polyetheramine at the percentage of grafting on nano-carbon material surface.
3. determine the content of carbonoxide material surface-COOH according to the principle of acid-base neutralisation reaction, determine the add-on of polyethex amine modification agent, effectively controlled the percentage of grafting of polyetheramine at carbon material surface.This also is innovative point of the present invention.
The present invention is take nanometer carbon black grafting aliphatic amine polyoxyethylene ether AC1860 as example, and behind the original nanometer carbon black oxidation purification, adopting the acid base titration principle to record oxidized black surface-COOH content is 3.58mmol/g.AC1860 is calculated as follows at the maximum percentage of grafting w (MAX) on 1g oxidized black OCB surface:
m(AC1860)?=3.58×10 -3×M(AC1860)=3.58×2.911=10.42g
w(MAX)=m(AC1860)÷(m(AC1860)+m(OCB))=10.42÷(10.42+1)=91.24%
According to calculation result, we can obtain the novel nano carbon black fluid of percentage of grafting between 75.00%-91.24% by the add-on of regulating AC1860.
Description of drawings
Fig. 1 is novel nano carbon fluid composition principle figure.
Embodiment
The present invention relates to the preparation method of a burst of novel nano carbon fluid, the method is: first original nano-carbon material is joined strongly-acid oxidation solution (V (dense H 2SO 4): V (dense HNO 3In the)=3:1), obtain the active oxidation carbon material of surperficial containing-COOH; Then under the condition of ultrasonic and magnetic agitation, take the polyetheramine that contains amido as properties-correcting agent, join in the active oxidation carbon material suspension, amido and carboxyl are finished the grafting of polyetheramine and carbonoxide material in polyetheramine and carbonoxide material interface generation acid-base reaction; By regulating type and the consumption of polyetheramine, obtain being under the room temperature polyethex amine modification carbon material particle of flow-like.The preparation method is simple for this nano-sized carbon fluid, is applicable to the synthetic of various carbon materials fluid.The carbon material particle that makes has nucleocapsid structure: examine and be carbon material, the polyetheramine shell by ionic linkage and carbon surface-COOH is connected.This structure is given the rheological property of carbon fluid uniqueness, namely is flow-like under the room temperature solvent-free condition, simultaneously by the type that changes polyetheramine and wetting ability and the lipophilicity that consumption can be regulated carbon material.This material has the applications well prospect aspect coating, plastics, rubber and the functional materials.
The invention will be further described below in conjunction with embodiment and accompanying drawing, but be not limited only to following case study on implementation.
Embodiment 1:
1) with dense H 2SO 4, dense HNO 33:1 is mixed with acidic oxidation liquid by volume, joins in the Erlenmeyer flask that fills original carbon black, obtains the oxidized black mixed solution; Mixed solution is ultrasonic complete to the carbon material oxidation, obtain the oxidized black reaction solution; With the oxidized black reaction solution dialyse, drying and processing, obtain the oxidized black particle, for subsequent use.
2) get the 0.2g oxidized black, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxidized black suspension again; Compound concentration is HCl, the NaOH solution of 0.01 mol/L, and excessive NaOH solution is added drop-wise in the carbonoxide material suspension, and reaction 24h obtains alkaline oxygenated carbon material suspension; Drip HCl in alkaline oxygenated carbon material suspension, measure acidity-basicity ph, stop titration when treating pH=7, calculate the content of black carbon surface acidic functionality-COOH.
3) oxidized black/polyether diamine graft reaction.Get the 1g oxidized black, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxidized black suspension again; Get an amount of (being determined by acid-base reaction) polyether diamine, be dissolved in the deionized water, obtain polyether diamine solution; Oxidized black suspension is slowly dripped in polyether diamine solution, obtain oxidized black/polyether diamine mixing solutions, magnetic agitation 2h, ultrasonic 30min continues magnetic agitation 48h and reacts completely to polyether diamine and oxidized black.Obtain oxidized black/polyether diamine reaction solution.
4) oven dry oxidized black/polyether diamine reaction solution obtains a kind of nanometer carbon black fluid.
Embodiment 2:
1) with dense H 2SO 4, dense HNO 33:1 is mixed with acidic oxidation liquid by volume, joins in the Erlenmeyer flask that fills original Graphene, obtains graphene oxide liquid mixture; Mixed solution is ultrasonic complete to the Graphene oxidation, obtain the graphene oxide reaction solution; With the graphene oxide reaction solution dialyse, drying and processing, obtain the graphene oxide particle, for subsequent use.
2) get the 0.2g graphene oxide, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed graphene oxide suspension again; Compound concentration is HCl, the NaOH solution of 0.01 mol/L, and excessive NaOH solution is added drop-wise in the graphene oxide suspension, and reaction 24h obtains alkaline oxygenated graphene suspension; Drip HCl in alkaline oxygenated graphene suspension, measure acidity-basicity ph, stop titration when treating pH=7, calculate Graphene surface acidity functional group-COOH content.
3) graphene oxide/polyether monoamine graft reaction.Get the 1g graphene oxide, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed graphene oxide suspension again; Get an amount of (being determined by acid-base reaction) polyether monoamine, be dissolved in the deionized water, obtain polyether monoamine solution; Graphene suspension is slowly dripped in polyether monoamine solution, obtain Graphene/polyether monoamine mixing solutions, magnetic agitation 2h, ultrasonic 30min continues magnetic agitation 48h and reacts completely to polyether monoamine and Graphene.Obtain Graphene/polyether monoamine reaction solution.
4) oven dry Graphene/polyether monoamine reaction solution obtains a kind of nano-graphene fluid.
Embodiment 3:
1) with dense H 2SO 4, dense HNO 33:1 is mixed with acidic oxidation liquid by volume, joins in the Erlenmeyer flask that fills original nano-graphite, obtains oxidized graphite mixed liquor; Mixed solution is ultrasonic complete to graphite oxidation, obtain the graphite oxide reaction solution; With the graphite oxide reaction solution dialyse, drying and processing, obtain the graphite oxide particle, for subsequent use.
2) get the 0.2g graphite oxide, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed graphite oxide suspension again; Compound concentration is HCl, the NaOH solution of 0.01 mol/L, and excessive NaOH solution is added drop-wise in the graphite oxide suspension, and reaction 24h obtains alkaline oxygenated graphite suspension; Drip HCl in alkaline oxygenated carbon material suspension, measure acidity-basicity ph, stop titration when treating pH=7, calculate the content of graphite surface acidic functionality-COOH.
3) graphite oxide/polyethers triamine graft reaction.Get the 1g graphite oxide, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed graphite oxide suspension again; Get an amount of (being determined by acid-base reaction) polyethers triamine, be dissolved in the deionized water, obtain the polyethers triamine solution; Graphite suspension is slowly dripped in the polyethers triamine solution, obtain Graphene/polyethers triamine mixing solutions, magnetic agitation 2h, ultrasonic 30min continues magnetic agitation 48h and reacts completely to polyethers triamine and graphite.Obtain graphite/polyethers triamine liquid.
4) oven dry graphite/polyethers triamine liquid obtains a kind of nano-graphite fluid.
Embodiment 4:
1) with dense H 2SO 4, dense HNO 33:1 is mixed with acidic oxidation liquid by volume, joins in the Erlenmeyer flask that fills original Nano diamond, obtains the oxidized diamond mixed solution; Mixed solution is ultrasonic complete to the diamond oxidation, obtain the oxidized diamond reaction solution; With the oxidized diamond reaction solution dialyse, drying and processing, obtain the oxidized diamond particle, for subsequent use.
2) get the 0.2g oxidized diamond, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxidized diamond suspension again; Compound concentration is HCl, the NaOH solution of 0.01 mol/L, and excessive NaOH solution is added drop-wise in the oxidized diamond suspension, and reaction 24h obtains alkaline oxygenated diamond suspension; Drip HCl in alkaline oxygenated diamond suspension, measure acidity-basicity ph, stop titration when treating pH=7, calculate the content of diamond surface acidic functionality-COOH.
3) oxidized diamond/polytetramethylene diethyl alcohol radical polyetheramine graft reaction.Get 1g carbonoxide material, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxidized diamond suspension again; Get an amount of (being determined by acid-base reaction) polytetramethylene diethyl alcohol radical polyetheramine, be dissolved in the deionized water, obtain polytetramethylene diethyl alcohol radical polyether amine solution; Diamond suspension is slowly dripped in polytetramethylene diethyl alcohol radical polyether amine solution, obtain diamond/polytetramethylene diethyl alcohol radical polyetheramine mixing solutions, magnetic agitation 2h, ultrasonic 30min continues magnetic agitation 48h and reacts completely to polytetramethylene diethyl alcohol radical polyetheramine and diamond.Obtain diamond/polytetramethylene diethyl alcohol radical polyetheramine reaction solution.
4) oven dry diamond/polytetramethylene diethyl alcohol radical polyetheramine reaction solution obtains a kind of Nano diamond fluid.
Embodiment 5:
1) with dense H 2SO 4, dense HNO 33:1 is mixed with acidic oxidation liquid by volume, joins in the Erlenmeyer flask that fills original carbon nanotube, obtains the oxide/carbon nanometer tube mixed solution; Mixed solution is ultrasonic complete to the carbon nanotube oxidation, obtain the oxide/carbon nanometer tube reaction solution; With the oxide/carbon nanometer tube reaction solution dialyse, drying and processing, obtain the oxide/carbon nanometer tube particle, for subsequent use.
2) get the 0.2g oxide/carbon nanometer tube, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxide/carbon nanometer tube suspension again; Compound concentration is HCl, the NaOH solution of 0.01 mol/L, and excessive NaOH solution is added drop-wise in the oxide/carbon nanometer tube suspension, and reaction 24h obtains alkaline oxygenated carbon nano tube suspension; Drip HCl in alkaline oxygenated carbon nano tube suspension, acidity-basicity ph to be determined stops titration when treating pH=7, calculates the content of carbon nano tube surface acidic functionality-COOH.
3) oxide/carbon nanometer tube/aliphatic amine polyoxyethylene ether graft reaction.Get the 1g oxide/carbon nanometer tube, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxide/carbon nanometer tube suspension again; Get an amount of (being determined by acid-base reaction) aliphatic amine polyoxyethylene ether, be dissolved in the deionized water, obtain aliphatic amine polyoxyethylene ether solution; Carbon nano tube suspension is slowly dripped in aliphatic amine polyoxyethylene ether solution, obtain carbon nanotube/aliphatic amine polyoxyethylene ether mixing solutions, magnetic agitation 2h, ultrasonic 30min continues magnetic agitation 48h and reacts completely to aliphatic amine polyoxyethylene ether and carbon nanotube.Obtain carbon nanotube/aliphatic amine polyoxyethylene ether reaction solution.
4) oven dry carbon nanotube/aliphatic amine polyoxyethylene ether reaction solution obtains a kind of carbon nanotube fluid.
Embodiment 6:
1) with dense H 2SO 4, dense HNO 33:1 is mixed with acidic oxidation liquid by volume, joins in the Erlenmeyer flask that fills original carbon nano fiber, obtains oxidation nanometer carbon fiber mixed solution; Mixed solution is ultrasonic complete to the carbon nano fiber oxidation, obtain oxidation nanometer carbon fiber reaction solution; With oxidation nanometer carbon fiber reaction solution dialyse, drying and processing, obtain oxidation nanometer carbon fiber particle, for subsequent use.
2) get 0.2g oxidation nanometer carbon fiber, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxidation nanometer carbon fiber suspension again; Compound concentration is HCl, the NaOH solution of 0.01 mol/L, and excessive NaOH solution is added drop-wise in the oxidation nanometer carbon fiber suspension, and reaction 24h obtains alkaline oxygenated carbon nano fiber suspension; Drip HCl in alkaline oxygenated carbon nano fiber suspension, acidity-basicity ph to be determined stops titration when treating pH=7, calculates the content of carbon nano fiber surface acidity functional group-COOH.
3) oxidation nanometer carbon fiber/aliphatic amine polyoxyethylene ether graft reaction.Get 1g oxidation nanometer carbon fiber, slowly be dissolved in the deionized water, magnetic agitation 2h, ultrasonic 30min, magnetic agitation 24h obtains finely dispersed oxidation nanometer carbon fiber suspension again; Get an amount of (being determined by acid-base reaction) aliphatic amine polyoxyethylene ether, be dissolved in the deionized water, obtain aliphatic amine polyoxyethylene ether solution; Carbon nano fiber suspension is slowly dripped in aliphatic amine polyoxyethylene ether solution, obtain carbon nano fiber/aliphatic amine polyoxyethylene ether mixing solutions, magnetic agitation 2h, ultrasonic 30min continues magnetic agitation 48h and reacts completely to aliphatic amine polyoxyethylene ether and carbon nano fiber.Obtain carbon nano fiber/aliphatic amine polyoxyethylene ether reaction solution.
4) oven dry carbon nano fiber/aliphatic amine polyoxyethylene ether reaction solution obtains a kind of carbon nano fiber fluid.
In above-described embodiment, described " carbonoxide material/polyetheramine " be polyethex amine modification carbonoxide material by name entirely, and the implication of wherein "/" is two integral parts of representative species, and/front portion is divided into the material that is modified, and/rear portion is divided into properties-correcting agent; The implication of "/" in other title material also is like this herein.

Claims (6)

1. the preparation method of a nano-sized carbon fluid is characterized in that first original nano-carbon material being joined in the strongly-acid oxidation solution, and the strongly-acid oxidation solution is V (dense H 2SO 4): V (dense HNO 3)=3:1, obtaining a kind of surface contains-the active oxidation carbon material of COOH; Then under the condition of ultrasonic and magnetic agitation, take the polyetheramine that contains amido as properties-correcting agent, join in the active oxidation carbon material suspension, amido and carboxyl are finished the grafting of polyetheramine and carbonoxide material in polyetheramine and carbonoxide material interface generation acid-base reaction; By regulating type and the consumption of polyetheramine, can obtain being under the room temperature polyethex amine modification carbon material particle of flow-like.
2. the preparation method of nano-sized carbon fluid according to claim 1 is characterized in that may further comprise the steps:
(1) carbonoxide material:
The vitriol oil, concentrated nitric acid are configured to the strongly-acid oxidation solution by proportioning, join in the Erlenmeyer flask that fills original carbon material, obtain carbonoxide material mixing liquid; Mixed solution is ultrasonic complete to the carbon material oxidation, obtain carbonoxide material reaction solution; With carbonoxide material reaction solution dialyse, drying and processing, obtain carbonoxide material particle, for subsequent use;
(2) acid functional mass contg assessment:
Configure rare HCl, dilute NaOH solution, utilize acid base titration principle assessment acidic functionality-COOH at the grafting content of carbon material surface;
(3) carbonoxide material/polyetheramine graft reaction:
Get an amount of carbonoxide material, be dispersed in the deionized water, obtain the carbonoxide material suspension; Determined the consumption of polyetheramine by the acid-base reaction principle, this polyetheramine is dissolved in the deionized water, obtain polyether amine solution; The carbon material hanging drop is fixed in the polyether amine solution, and ultrasonic agitation to carbonoxide material and polyetheramine reacts completely, and obtains carbonoxide material/polyetheramine reaction solution;
(4) oven dry carbonoxide material/polyetheramine reaction solution;
Through above-mentioned steps, obtain described nano-sized carbon fluid.
3. the preparation method of nano-fluid carbon material according to claim 2 is characterized in that described original nano-carbon material adopts nanometer carbon black, nano-graphite, Nano diamond, Graphene, carbon nanotube or carbon nano fiber.
4. the preparation method of nano-fluid carbon material according to claim 2 is characterized in that the dense H described in the step (1) 2SO 4Mass concentration be 98%, described dense HNO 3Mass concentration be 68%.
5. the preparation method of nano-fluid carbon material according to claim 2 is characterized in that the concentration of the rare HCl described in the step (2) and rare NaOH is 0.01 mol/L.
6. the preparation method of nano-fluid carbon material according to claim 2 is characterized in that: described polyetheramine employing polyether monoamine, polyether diamine, polyethers triamine, polytetramethylene diethyl alcohol radical polyetheramine or aliphatic amine polyoxyethylene ether.
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CN105906842A (en) * 2016-04-29 2016-08-31 四川大学 Modified graphene oxide and epoxy resin composite material and method for preparing same
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CN107154498B (en) * 2017-05-17 2020-05-19 华中科技大学 Preparation method and application of microporous carbon structure electrode material prepared from plant material
CN109054791A (en) * 2018-07-16 2018-12-21 中国石油大学(华东) A kind of water base carbon nanofluid and preparation method thereof
CN109054791B (en) * 2018-07-16 2020-10-16 中国石油大学(华东) Water-based carbon nanofluid and preparation method thereof
CN111410855A (en) * 2019-12-31 2020-07-14 宁波德泰化学有限公司 Preparation method of high-surface-activity/high-hydrophilicity dispersion type carbon black
CN111334044A (en) * 2020-04-22 2020-06-26 中国工程物理研究院电子工程研究所 Organic silicone gel for precise electronic component encapsulation and use method thereof

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Application publication date: 20130213