CN104211053A - Preparation method of modified graphene aqueous dispersion - Google Patents

Preparation method of modified graphene aqueous dispersion Download PDF

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Publication number
CN104211053A
CN104211053A CN201410445881.8A CN201410445881A CN104211053A CN 104211053 A CN104211053 A CN 104211053A CN 201410445881 A CN201410445881 A CN 201410445881A CN 104211053 A CN104211053 A CN 104211053A
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China
Prior art keywords
modified graphene
preparation
graphene oxide
aqueous dispersions
graphene
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CN201410445881.8A
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Chinese (zh)
Inventor
王圆圆
崔璨
孙明娟
侯士峰
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JINING LEADER NANO TECHNOLOGY Co Ltd
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JINING LEADER NANO TECHNOLOGY Co Ltd
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Priority to CN201410445881.8A priority Critical patent/CN104211053A/en
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Abstract

The invention discloses a preparation method of a modified graphene aqueous dispersion. The preparation method comprises the following steps: preparing graphene oxide slurry and cleaning the graphene oxide slurry to be neutral; covalently modifying by virtue of surfactants such as polyvinylpyrrolidone, polyoxyethylene and sodium polystyrenesulfonate; then, obtaining graphene which is covalently modified by surfactants such as polyvinylpyrrolidone in one step by means of a reducing action; and carrying out ultrasonic dispersion to obtain the modified graphene aqueous dispersion. The modified graphene aqueous dispersion disclosed by the invention is high in stability, good in dispersibility, low in production cost and simple in process. The required equipment is simple, the yield is high and industrialized production is easy to realize.

Description

A kind of preparation method of modified graphene aqueous dispersions
Technical field
The invention belongs to technical field of graphene, relate in particular to a kind of preparation method of high stability modified graphene aqueous dispersions.
Background technology
Graphene has lot of superiority energy as a kind of type material, as high in intensity, good conductivity, high-specific surface area, excellent heat conductivity etc.; Thus potential using value is had in high-performance nano electron device, field emmision material, reserves and sensor field.But due to the high-specific surface area of Graphene, there is Van der Waals force in grapheme material between layers, thus easily reunites; In actual applications, grapheme material needs dispersion in a solvent, but grapheme material is reunited in a large number, thus is difficult to be scattered in all kinds of SOLVENTS, greatly limit its application.
Be typically employed in prior art in aqueous povidone solution to be peeled off by the liquid phase of graphite and prepare water-soluble graphene, or by supersound process powdered graphite, the aqueous solution adjoining pyrrolidone at polyethylene utilizes the sterically hindered of nonionic hydrophilic high mol and vacancy stabilization, obtain water miscible single-layer graphene, and then obtained high-quality graphene dispersion liquid, but it is lower to obtain single-layer graphene productive rate by these methods.
Summary of the invention
The object of the present invention is to provide a kind of method preparing modified graphene aqueous dispersions, make prepare Graphene aqueous dispersions stability high, good dispersity, output are high, be easy to realize suitability for industrialized production.
The present invention solves the technical scheme that its technical problem takes: a kind of preparation method of modified graphene aqueous dispersions, is characterized in that: it comprises the following steps:
(1) graphene oxide slurry is obtained by reacting with natural graphite and strong oxidizer;
(2) get a certain amount of graphene oxide slurry, cleaning is to neutral;
(3) dried by graphene oxide, compound concentration is the graphene oxide water solution of 0.005 ~ 0.01g/mL;
(4) in graphene oxide water solution, tensio-active agent is added;
(5) carry out magnetic agitation, mix;
(6) add a certain amount of reductive agent, carry out oil bath reaction when magnetic agitation, suction filtration obtains modified graphene;
(7) modified graphene is added the distilled water of certain volume, carry out ultrasonic disperse, ultrasonic power 50-150w, ultrasonic time 2-6h, be mixed with certain density modified graphene aqueous dispersions.
Graphene oxide described in step (4) and the mass ratio of tensio-active agent are 1:5-5:1.
Described tensio-active agent is one or more mixture of polyvinylpyrrolidone, polyoxyethylene, sodium polystyrene sulfonate, Sodium dodecylbenzene sulfonate.
The molecular weight 200-20 ten thousand of above-mentioned polyvinylpyrrolidone, polyoxyethylene 800-800 ten thousand.
Described reductive agent is a kind of or above-mentioned two or more mixture of hydrazine hydrate, the acid of anti-sepsis, sodium borohydride.
The invention has the beneficial effects as follows: the present invention selects graphene oxide to be starting raw material, utilize polyethylene to adjoin good water-soluble of the tensio-active agents such as pyrrolidone, obtain dispersed Graphene preferably in aqueous material modified-modified graphene aqueous dispersions; The modified graphene aqueous dispersions good stability utilizing the method to prepare, output are high, are easy to realize suitability for industrialized production.
Embodiment
Technical scheme of the present invention is further illustrated below by specific embodiment.
embodiment 1
(1) get 1g natural graphite and strong oxidizer potassium permanganate, 98% vitriol oil 10ml, solution reaction temperature controls below 40 degree, and stirring reaction 3 hours, obtains graphene oxide slurry;
(2) get above-mentioned graphene oxide slurry 1g, adopt the mode of washing to clean to neutrality;
(3) cleaning is obtained graphene oxide after drying to neutral graphene oxide slurry, be mixed with the graphene oxide water solution 100mL of 0.005g/mL concentration;
(4) in above-mentioned graphene oxide water solution, 0.1g polyvinylpyrrolidone is added;
(5) magnetic agitation, mixes;
(6) add the anti-sepsis acid of 1.0g again, under the condition of magnetic agitation, oil bath is reacted, and controlling temperature of reaction is 90 degree, reaction 3h;
(7), after reaction terminates, suction filtration, obtains the Graphene of polyvinyl pyrrolidone modified;
(8) by the Graphene of modification, add the distilled water of certain volume, carry out ultrasonic disperse, ultrasonic power 150w, ultrasonic time 2h, be mixed with certain density modified graphene aqueous dispersions.
The modified graphene aqueous dispersions configured is more stable, and placing bottom after month, still can stable existence without any precipitation.
embodiment 2
(1) get 1g natural graphite and strong oxidizer potassium permanganate 1g, 98% vitriol oil 10ml, solution reaction temperature controls below 30 degree, and stirring reaction 3 hours, obtains graphene oxide slurry;
(2) get above-mentioned graphene oxide slurry 1g, adopt the mode of washing to clean to neutrality;
(3) cleaning is obtained graphene oxide after drying to neutral graphene oxide slurry, be mixed with the graphene oxide water solution 100mL of 0.01g/mL concentration;
(4) in graphene oxide water solution, 5g sodium polystyrene sulfonate is added;
(5) magnetic agitation, mixes;
(6) add the anti-sepsis acid of 1.5g, under the condition of magnetic agitation, oil bath is reacted;
(7), after reaction terminates, suction filtration, obtains the Graphene of sodium polystyrene sulfonate modification.
(8) by the Graphene of modification, add the distilled water of certain volume, carry out ultrasonic disperse, ultrasonic power 50w, ultrasonic time 6h, be mixed with certain density modified graphene aqueous dispersions.

Claims (5)

1. a preparation method for modified graphene aqueous dispersions, is characterized in that: it comprises the following steps:
(1) graphene oxide slurry is obtained by reacting with natural graphite and strong oxidizer;
(2) get a certain amount of graphene oxide slurry, cleaning is to neutral;
(3) dried by graphene oxide slurry, compound concentration is the graphene oxide water solution of 0.005 ~ 0.01 g/mL;
(4) in above-mentioned graphene oxide water solution, tensio-active agent is added;
(5) magnetic agitation, mixes;
(6) add a certain amount of reductive agent, carry out oil bath reaction when magnetic agitation, suction filtration obtains modified graphene;
(7) in modified graphene, add the distilled water of certain volume again, carry out ultrasonic disperse, ultrasonic power 50-150w, ultrasonic time 2-6h, be mixed with certain density modified graphene aqueous dispersions.
2. the preparation method of a kind of modified graphene aqueous dispersions according to claim 1, is characterized in that the mass ratio of described graphene oxide and tensio-active agent is 1:5-5:1.
3. the preparation method of a kind of modified graphene aqueous dispersions according to claim 1, is characterized in that: described tensio-active agent is one or more mixture of polyvinylpyrrolidone, polyoxyethylene, sodium polystyrene sulfonate, Sodium dodecylbenzene sulfonate.
4. the preparation method of a kind of modified graphene aqueous dispersions according to claim 1, is characterized in that: the molecular weight 200-200 ten thousand of described polyvinylpyrrolidone, sodium polystyrene sulfonate, polyoxyethylene 800-80 ten thousand.
5. the preparation method of a kind of modified graphene aqueous dispersions according to claim 1, is characterized in that: described reductive agent is a kind of or above-mentioned two or more mixture of hydrazine hydrate, the acid of anti-sepsis, sodium borohydride.
CN201410445881.8A 2014-09-04 2014-09-04 Preparation method of modified graphene aqueous dispersion Pending CN104211053A (en)

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Cited By (21)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104558708A (en) * 2015-01-19 2015-04-29 南京理工大学 Multifunctional vulcanized rubber containing polyvinylpyrrolidone-modified graphene oxide and preparation method of multifunctional vulcanized rubber
CN104677846A (en) * 2015-02-28 2015-06-03 济宁利特纳米技术有限责任公司 Quantitative analysis method for graphene dispersion liquid
CN104716322A (en) * 2015-03-17 2015-06-17 济宁利特纳米技术有限责任公司 Preparation method for modified graphene and application of modified graphene to positive materials for lithium batteries
CN105752971A (en) * 2016-03-30 2016-07-13 成都新柯力化工科技有限公司 Nano-graphene material special for drug carrier and preparing method
CN106057495A (en) * 2016-05-18 2016-10-26 哈尔滨万鑫石墨谷科技有限公司 Super capacitor flexible electrode, preparation method and super capacitor
CN106276867A (en) * 2016-07-21 2017-01-04 绍兴文理学院 The photoelectric modified graphene of a kind of enhancing
CN106328256A (en) * 2016-10-28 2017-01-11 济宁利特纳米技术有限责任公司 Conductive slurry for lithium ion battery and preparation method of conductive slurry
CN106433593A (en) * 2016-08-26 2017-02-22 河南正佳能源环保股份有限公司 Preparation method for graphene nano oil displacement agent
CN106752833A (en) * 2017-01-19 2017-05-31 青岛大学 A kind of preparation method of graphene oxide/silica composite coating
CN107285301A (en) * 2017-08-17 2017-10-24 济宁利特纳米技术有限责任公司 A kind of high concentration graphene dispersion liquid and preparation method thereof
CN107591540A (en) * 2017-08-27 2018-01-16 长沙小新新能源科技有限公司 A kind of preparation method of biological fuel cell anode material
CN108394892A (en) * 2018-05-11 2018-08-14 西安交通大学 A kind of graphene dispersion liquid and preparation method thereof that directly graphene is modified
CN108726513A (en) * 2018-09-05 2018-11-02 广东墨睿科技有限公司 A kind of preparation method of graphene dispersing solution
CN108997867A (en) * 2018-09-17 2018-12-14 深圳市心版图科技有限公司 A kind of Environmental Protective Water-paint and preparation method thereof
CN109082728A (en) * 2017-06-13 2018-12-25 山东圣泉新材料股份有限公司 A kind of vegetable protein nanofiber and preparation method thereof containing graphene
CN109368629A (en) * 2018-12-03 2019-02-22 广东电网有限责任公司 A kind of graphene dispersion system and preparation method thereof
CN109575642A (en) * 2019-01-21 2019-04-05 中北大学 It is a kind of can again oiliness dispersion modified graphene raw powder's production technology
CN109666259A (en) * 2017-10-16 2019-04-23 山东欧铂新材料有限公司 A kind of preparation method of modified graphene oxide, modified graphene and modified graphene epoxy resin dispersion liquid
CN109824045A (en) * 2019-03-22 2019-05-31 西安交通大学 A kind of graphene dispersing solution and preparation method thereof of direct modified graphene preparation
CN110498634A (en) * 2019-08-02 2019-11-26 广西科技大学 A kind of graphene aqueous dispersions, graphene concrete and preparation method thereof
CN112011137A (en) * 2019-05-13 2020-12-01 中国科学院化学研究所 Graphene/water-soluble polymer composite material and preparation method thereof

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CN103935994A (en) * 2014-04-28 2014-07-23 上海交通大学 Self-supported reduced graphene oxide paper and preparation method thereof
CN103979531A (en) * 2014-05-22 2014-08-13 天津大学 Application of electrochemical sensor prepared from graphene material in bisphenol A detection

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CN102502612A (en) * 2011-11-21 2012-06-20 南京工业大学 Method for preparing grapheme through oxidation reduction
CN102659099A (en) * 2012-05-29 2012-09-12 上海第二工业大学 Preparation method of anisotropic graphene foam
DE102012216828A1 (en) * 2012-09-19 2014-03-20 Sgl Carbon Se Producing modified graphene oxide useful in a composite material used as e.g. electrical insulation material for electrical and combustion components in e.g. computer, comprises mixing graphene oxide and surfactant
CN103935994A (en) * 2014-04-28 2014-07-23 上海交通大学 Self-supported reduced graphene oxide paper and preparation method thereof
CN103979531A (en) * 2014-05-22 2014-08-13 天津大学 Application of electrochemical sensor prepared from graphene material in bisphenol A detection

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104558708A (en) * 2015-01-19 2015-04-29 南京理工大学 Multifunctional vulcanized rubber containing polyvinylpyrrolidone-modified graphene oxide and preparation method of multifunctional vulcanized rubber
CN104677846A (en) * 2015-02-28 2015-06-03 济宁利特纳米技术有限责任公司 Quantitative analysis method for graphene dispersion liquid
CN104716322A (en) * 2015-03-17 2015-06-17 济宁利特纳米技术有限责任公司 Preparation method for modified graphene and application of modified graphene to positive materials for lithium batteries
CN105752971A (en) * 2016-03-30 2016-07-13 成都新柯力化工科技有限公司 Nano-graphene material special for drug carrier and preparing method
CN106057495A (en) * 2016-05-18 2016-10-26 哈尔滨万鑫石墨谷科技有限公司 Super capacitor flexible electrode, preparation method and super capacitor
CN106057495B (en) * 2016-05-18 2019-01-18 哈尔滨万鑫石墨谷科技有限公司 A kind of supercapacitor flexible electrode, preparation method and supercapacitor
CN106276867A (en) * 2016-07-21 2017-01-04 绍兴文理学院 The photoelectric modified graphene of a kind of enhancing
CN106433593A (en) * 2016-08-26 2017-02-22 河南正佳能源环保股份有限公司 Preparation method for graphene nano oil displacement agent
CN106328256A (en) * 2016-10-28 2017-01-11 济宁利特纳米技术有限责任公司 Conductive slurry for lithium ion battery and preparation method of conductive slurry
CN106752833A (en) * 2017-01-19 2017-05-31 青岛大学 A kind of preparation method of graphene oxide/silica composite coating
CN109082728B (en) * 2017-06-13 2021-03-12 山东圣泉新材料股份有限公司 Graphene-containing plant protein nanofiber and preparation method thereof
CN109082728A (en) * 2017-06-13 2018-12-25 山东圣泉新材料股份有限公司 A kind of vegetable protein nanofiber and preparation method thereof containing graphene
CN107285301A (en) * 2017-08-17 2017-10-24 济宁利特纳米技术有限责任公司 A kind of high concentration graphene dispersion liquid and preparation method thereof
CN107591540A (en) * 2017-08-27 2018-01-16 长沙小新新能源科技有限公司 A kind of preparation method of biological fuel cell anode material
CN109666259A (en) * 2017-10-16 2019-04-23 山东欧铂新材料有限公司 A kind of preparation method of modified graphene oxide, modified graphene and modified graphene epoxy resin dispersion liquid
CN109666259B (en) * 2017-10-16 2022-05-27 山东欧铂新材料有限公司 Preparation method of modified graphene oxide, modified graphene and modified graphene epoxy resin dispersion liquid
CN108394892A (en) * 2018-05-11 2018-08-14 西安交通大学 A kind of graphene dispersion liquid and preparation method thereof that directly graphene is modified
CN108726513A (en) * 2018-09-05 2018-11-02 广东墨睿科技有限公司 A kind of preparation method of graphene dispersing solution
CN108997867A (en) * 2018-09-17 2018-12-14 深圳市心版图科技有限公司 A kind of Environmental Protective Water-paint and preparation method thereof
CN109368629A (en) * 2018-12-03 2019-02-22 广东电网有限责任公司 A kind of graphene dispersion system and preparation method thereof
CN109575642A (en) * 2019-01-21 2019-04-05 中北大学 It is a kind of can again oiliness dispersion modified graphene raw powder's production technology
CN109824045A (en) * 2019-03-22 2019-05-31 西安交通大学 A kind of graphene dispersing solution and preparation method thereof of direct modified graphene preparation
CN112011137A (en) * 2019-05-13 2020-12-01 中国科学院化学研究所 Graphene/water-soluble polymer composite material and preparation method thereof
CN112011137B (en) * 2019-05-13 2021-10-08 中国科学院化学研究所 Graphene/water-soluble polymer composite material and preparation method thereof
CN110498634A (en) * 2019-08-02 2019-11-26 广西科技大学 A kind of graphene aqueous dispersions, graphene concrete and preparation method thereof

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Inventor after: Wang Yuanyuan

Inventor after: Cui Can

Inventor after: Sun Mingjuan

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Inventor before: Cui Can

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Inventor before: Hou Shifeng

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Application publication date: 20141217