CN107935032A - A kind of preparation method of the graphene-based conductive titanium dioxide of high dispersive type - Google Patents

A kind of preparation method of the graphene-based conductive titanium dioxide of high dispersive type Download PDF

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CN107935032A
CN107935032A CN201810004878.0A CN201810004878A CN107935032A CN 107935032 A CN107935032 A CN 107935032A CN 201810004878 A CN201810004878 A CN 201810004878A CN 107935032 A CN107935032 A CN 107935032A
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graphene
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titanium dioxide
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ultrasonically treated
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CN107935032B (en
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鄂涛
钱建华
杨姝宜
刘琳
邢锦娟
李莹
马丹
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Fuxin Feixiang leather products Co.,Ltd.
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Bohai University
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    • C01—INORGANIC CHEMISTRY
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    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract

The present invention discloses a kind of preparation method of the graphene-based conductive titanium dioxide of high dispersive type, implements successively as follows：1）Titanium dioxide is added in beaker, deionized water is added and is disperseed, titania solution is made；The polyglycol solution of titanium dioxide is added, adjusts pH value of solution；It is ultrasonically treated；Continue and be stirred；2）Weigh certain mass percentage graphene；The graphene is added in neopelex solution, is ultrasonically treated；Graphene solution is added to step 1）In, it is ultrasonically treated；3）Cationic-type polyacrylamide solution is configured, is ultrasonically treated；Polyacrylamide solution is added drop-wise to step 2）In；4）After reaction, pH is adjusted, is ultrasonically treated, up to purpose product.The object of the invention product not only has high conductivity, but also with the polymolecularity in aqueous solution, can directly be applied in water paint and antistatic material, will not produce secondary pollution, cost is relatively low.

Description

A kind of preparation method of the graphene-based conductive titanium dioxide of high dispersive type
Technical field
The invention belongs to conductive titanium dioxide preparation method field, more particularly to a kind of electrically-conducting paint, antistatic high dispersive type The preparation method of graphene-based conductive titanium dioxide.
Background technology
Titanium dioxide is the basic material of the national economic development, and Aeronautics and Astronautics, automobile, machine-building, electric power, communicate, build Build, most industries such as household electrical appliances it is all basic by production of titanium dioxide.Prominent with modern chemical industry, agricultural and science and technology flies suddenly Into status of the titanium dioxide in human development is more and more important.Counted according to employer's organization, titanium dioxide enterprise of China is total within 2016 259.72 ten thousand tons of titanium dioxide is produced, increases by 11.8% on a year-on-year basis, wherein conductive titanium dioxide is widely used in electromagnetic shielding, antistatic Material, gas sensor, infrared absorption heat-barrier material and electrode material etc., are a kind of extremely potential novel conductive materials [Qian Liu, Liang Zhang, Jian-FengChen, YuanLe. Synthesis of TiO2@ATO core– shell nanofibers using coaxial electrospinning [J]. Materials Letters, 2014, 137: 339–342.]。
At present, conductive titanium dioxide generally use ATO methods are made.The preparation flow of ATO type composite conductive powders usually first will Carrier progress is pre-dispersed, then using liquid phase method（Such as chemical precipitation method, alkoxide process and evaporation）Carry out metal oxide Coat, be filtered, washed and dried roasting.Chemical precipitation method extensive use in the industrial production, such as Y. Wang [Ying Wang, Ji Zheng, Fei Jiang, Meng Zhang. Synthesis and conductive performance of antimony-doped tin oxide-coated TiO2 by the co-precipitation method [J]. J Mater Sci: Mater Electron, 2014, 25:4524-4530.] using titanium dioxide as matrix, Sb has been synthesizedxSn1- xO2Particle is 25nm, and resistivity is 2.546 × 103Sb-the SnO of Ω cm2/TiO2Composite conductive powder；This seminar also leads at the same time Cross TiO of the optimization reaction condition synthesis particle uniform particle size size in 8nm or so2/SbxSn1-xO2Composite conductive powder, its resistivity For 18 Ω cm [money Jian Hua, Sun Ke, Liu Lin, Xing Jinjuan, conductive TiO2The preparation of powder and performance study [J], chemistry is ground Study carefully and apply, 2016,28（3）: 350-354.].ATO methods prepare add during conductive titanium dioxide conductive agent amount it is general For TiO230% or so of quality, with high costs, resource consumption is big, during which produces substantial amounts of spent acid, salkali waste, does not meet country Environmental requirement, seriously constrains the popularization and application of conductive titanium dioxide.
The graphene electron mobility to receive much concern in recent years can reach 2 × 105cm2Electron mobility in/V s, about silicon 140 times, 20 times of GaAs, resistivity ratio copper or silver it is also low, be only 10-6Ω cm, are conductive best materials at room temperature Material.Therefore, prepare conductive titanium dioxide using the excellent electric conductivity of graphene and have a vast market prospect and important reality Meaning.
The content of the invention
The present invention is intended to provide a kind of preparation method of the graphene-based conductive titanium dioxide of high dispersive type, the titanium dioxide both had High conductivity, but with the polymolecularity in aqueous solution, the graphene-based conductive titanium dioxide prepared using the present invention can be direct Applied in water paint and antistatic material, secondary pollution will not be produced, cost is relatively low, easy to operate.
To reach above-mentioned purpose, the technical solution adopted by the present invention is.
The preparation method of the graphene-based conductive titanium dioxide of high dispersive type, can implement successively as follows.
（1）Titanium dioxide is added in beaker, deionized water is added and is disperseed, titania solution is made；Add two The polyglycol solution of titanium oxide, adjustment pH value of solution are 1~4；It is ultrasonically treated；Continue and be transferred in three-necked flask, carry out Stirring.
（2）By step（1）The titanium dioxide of middle certain mass percentage weighs graphene；The graphene is added to ten In dialkyl benzene sulfonic acids sodium solution, it is ultrasonically treated；Graphene solution is added to step（1）In, it is ultrasonically treated, is connect It is continuous to be stirred.
（3）Cationic-type polyacrylamide solution is configured, is ultrasonically treated；Polyacrylamide solution is added drop-wise to step （2）In.
（4）After reaction, pH is adjusted, is ultrasonically treated, up to the graphene-based conductive titanium dioxide of high dispersive type.
As a preferred embodiment, step of the present invention（1）In, the titanium dioxide that particle diameter is 20~500nm is added In beaker, add 100ml deionized waters and disperseed, the solution that mass concentration is 2%~60% is made；Add titanium dioxide quality 0.5%~3% polyglycol solution；It is ultrasonically treated in 400~1200W power brackets, 10~60min of ultrasonic time, Mixing speed is 600r/min.
Further, step of the present invention（2）In, by titanium dioxide mass percent graphene is weighed for 3%~15%； The resistivity of the graphene is less than 10-3Ω•cm；Average thickness is 5~10nm；Average piece footpath is 500nm~20 μm.
Further, step of the present invention（2）In, continue and the graphene is added to mass concentration as 5%~30% Neopelex solution in, be ultrasonically treated in 500~1200W power brackets, ultrasonic time 30~ 180min；The graphene solution is added to step（1）In, it is ultrasonically treated in 100~300W power brackets, ultrasound 2~24h of time, stirs 60min.
Further, step of the present invention（3）In, configuration concentration is 0.5%~5%, molecular weight be 500~10,000,000 it Between cationic-type polyacrylamide solution, hydrolyze 10~60min；Ultrasound is carried out in 200~800W power brackets, when ultrasonic Between 10~60min；Polyacrylamide solution is added drop-wise to by step using peristaltic pump（2）In, it is added dropwise to complete in 30~120min, with 800 r/min speed stir 1h.
Further, step of the present invention（4）In, after reaction, it is 1~4 to adjust pH；In 200~600W power In the range of carry out ultrasound, 30~180min of ultrasonic time, filter, 40~120 DEG C drying, under nitrogen protection, using air-flow Pulverizer handles it, obtains the graphene-based conductive titanium dioxide of high dispersive type that particle diameter is 200~500nm.
The present invention will be by controlling TiO2Electrically, TiO is adsorbed in graphene surface2, then using polyacrylamide to its into Row parcel, is prepared for graphene-based conductive titanium dioxide, graphene and TiO in this conductive titanium dioxide2In ultrasound and surfactant Under the action of, make its fully dispersed mixing, after polyacrylamide is added dropwise, network " bridge formation " effect, graphite are produced between particle Alkene passes through active force and the TiO such as " bridge formation ", bonding, adsorption, hydrogen bond2Stable bond, referring to attached drawing 1, formed graphene/ TiO2Bulky grain, it is finally small in the effect of airslide disintegrating mill, by graphene/TiO2It is 200~500nm that bulky grain, which cuts into particle diameter, Little particle.Experiment measures the graphene-based conductive titanium dioxide of the present invention, resistivity in the Ω cm of 0.875 Ω cm~83.457, Dispersion performance is good in aqueous solution, and 48h is not settled, and whiteness is specifically shown in Table 1 between 22~65 degree, will not produce secondary pollution, Financial cost is low, easy to operate, stable.
The property of 1 graphene Different adding amount conductive titanium dioxide of table.
Brief description of the drawings
Below in conjunction with specific embodiment, the invention will be further described.It is necessarily pointed out that the present embodiment is only For illustration, protection scope of the present invention does not limit to illustration category.
Fig. 1 is graphene of the present invention and TiO2Compound preceding SEM figures.
Fig. 2 is graphene of the present invention and TiO2SEM figures after compound.
Embodiment
Embodiment 1.
1）By the titanium dioxide that particle diameter is 20nm（TiO2）Add in beaker, add 100 ml deionized waters and disperseed, The solution that mass concentration is 2% is made, adds TiO2The polyethylene glycol of quality 0.5%, adjustment pH value of solution is 1, under 400W power Ultrasound is carried out, ultrasonic time 10min, is transferred in three-necked flask, is stirred with 600r/min.
2）Weigh step 1）Middle TiO2Mass fraction is 3% graphene（It is highly conductive, suboxides group, thickness 5~ 10nm, piece footpath 500nm~20 μm）, it is added in the neopelex solution that mass concentration is 5%, under 500W power Ultrasound is carried out, ultrasonic time 30min, step 1 is added to by graphene solution）In, ultrasound is carried out under 100W power, when ultrasonic Between 2h, stir 60min.
3）Configuration concentration is 0.5% cationic-type polyacrylamide（Molecular weight is 500~10,000,000）Solution, hydrolysis 10min, carries out ultrasound, ultrasonic time 10min, step is added drop-wise to using peristaltic pump by polyacrylamide solution under 200W power 2）In, it is added dropwise to complete in 30min, with 800r/min, stirs 1h.
4）After reaction, it is 4 to adjust pH value, ultrasound is carried out under 200W power, ultrasonic time 30min, filters, 40 DEG C drying, under nitrogen protection, handles it using airslide disintegrating mill, obtains the graphene-based conductive titanium white that particle diameter is 200nm Powder.
Embodiment 2.
1）By the titanium dioxide that particle diameter is 100nm（TiO2）Add in beaker, add 100 ml deionized waters and disperseed, The solution that mass concentration is 10% is made, adds TiO2The polyethylene glycol of quality 1%, adjustment pH value of solution is 3, under 600 W power Ultrasound is carried out, ultrasonic time 20min, is transferred in three-necked flask, is stirred with 600r/min.
2）Weigh 1）Middle TiO2Mass fraction is 4% graphene（It is highly conductive, suboxides group, 5~10nm of thickness, piece footpath 500nm~20 μm）, it is added in the neopelex solution that concentration is 8%, ultrasound is carried out under 600 W power, surpasses Sound time 60min, 1 is added to by graphene solution）In, ultrasound, ultrasonic time 4h, stirring are carried out in 150 W power brackets 60min。
3）Configuration concentration is 1% cationic-type polyacrylamide（Molecular weight is 500~10,000,000）Solution, hydrolysis 10~ 60min, carries out ultrasound, ultrasonic time 20min, 2 are added drop-wise to using peristaltic pump by polyacrylamide solution under 300W power） In, it is added dropwise to complete in 50min, with 800r/min, stirs 1h.
4）After reaction, it is 2 to adjust pH value, ultrasound is carried out under 300W power, ultrasonic time 40min, filters, 50 DEG C drying, under nitrogen protection, handles it using airslide disintegrating mill, obtains the graphene-based conductive titanium white that particle diameter is 250nm Powder.
Embodiment 3.
1）By the titanium dioxide that particle diameter is 200nm（TiO2）Add in beaker, add 100 ml deionized waters and disperseed, The solution that mass concentration is 20% is made, adds TiO2The polyethylene glycol of quality 1.5%, adjustment pH value of solution is 2, in 800 W power Lower to carry out ultrasound, ultrasonic time 30min, is transferred in three-necked flask, is stirred with 600r/min.
2）Weigh 1）Middle TiO2Mass fraction is 6% graphene（It is highly conductive, suboxides group, 5~10nm of thickness, piece footpath 500nm~20 μm）, it is added in the neopelex solution that concentration is 16%, ultrasound is carried out under 750W power, surpasses Sound time 90min, 1 is added to by graphene solution）In, ultrasound, ultrasonic time 10h, stirring are carried out in 200 W power brackets 60min。
3）Configuration concentration is 2% cationic-type polyacrylamide（Molecular weight is 500~10,000,000）Solution, hydrolysis 30min, carries out ultrasound, ultrasonic time 30min, 2 are added drop-wise to using peristaltic pump by polyacrylamide solution under 400W power） In, it is added dropwise to complete in 70min, with 800r/min, stirs 1h.
4）After reaction, it is 3 to adjust pH value, ultrasound is carried out under 400W power, ultrasonic time 80min, filters, 70 DEG C drying, under nitrogen protection, handles it using airslide disintegrating mill, obtains the graphene-based conductive titanium white that particle diameter is 300nm Powder.
Embodiment 4.
1）By the titanium dioxide that particle diameter is 300nm（TiO2）Add in beaker, add 100 ml deionized waters and disperseed, The solution that mass concentration is 30% is made, adds TiO2The polyethylene glycol of quality 2%, adjustment pH value of solution is 3, under 1000 W power Ultrasound is carried out, ultrasonic time 40min, is transferred in three-necked flask, is stirred with 600r/min.
2）Weigh 1）Middle TiO2Mass fraction is 8% graphene（It is highly conductive, suboxides group, 5~10nm of thickness, piece footpath 500nm~20 μm）, it is added in the neopelex solution that concentration is 20%, ultrasound is carried out under 900W power, surpasses Sound time 120min, 1 is added to by graphene solution）In, ultrasound is carried out in 250 W power brackets, ultrasonic time 16h, is stirred Mix 60min.
3）Configuration concentration is 3% cationic-type polyacrylamide（Molecular weight is 500~10,000,000）Solution, hydrolysis 40min, carries out ultrasound, ultrasonic time 40min, 2 are added drop-wise to using peristaltic pump by polyacrylamide solution under 500W power） In, it is added dropwise to complete in 90min, with 800r/min, stirs 1h.
4）After reaction, it is 2 to adjust pH value, and ultrasound is carried out under 500W power, and ultrasonic time 120min, filters, 90 DEG C of drying, under nitrogen protection, are handled it using airslide disintegrating mill, obtain the graphene-based conductive titanium that particle diameter is 350nm White powder.
Embodiment 5.
1）By the titanium dioxide that particle diameter is 400nm（TiO2）Add in beaker, add 100 ml deionized waters and disperseed, The solution that mass concentration is 40% is made, adds TiO2The polyethylene glycol of quality 2.5%, adjustment pH value of solution is 2, in 1100W power Lower to carry out ultrasound, ultrasonic time 50min, is transferred in three-necked flask, is stirred with 600r/min.
2）Weigh 1）Middle TiO2Mass fraction is 15% graphene（It is highly conductive, suboxides group, 5~10nm of thickness, piece Footpath 500nm~20 μm）, it is added in the neopelex solution that concentration is 25%, ultrasound is carried out under 1000W power, Ultrasonic time 150min, 1 is added to by graphene solution）In, ultrasonic, ultrasonic time 20h is carried out in 300 W power brackets, Stir 60min.
3）Configuration concentration is 4% cationic-type polyacrylamide（Molecular weight is 500~10,000,000）Solution, hydrolysis 50min, carries out ultrasonic, ultrasonic time 50min under 600W power, polyacrylamide solution is added drop-wise to 2 using peristaltic pump） In, it is added dropwise to complete in 110min, with 800r/min, stirs 1h.
4）After reaction, it is 3 to adjust pH value, and ultrasound is carried out under 500W power, and ultrasonic time 160min, filters, 100 DEG C of drying, under nitrogen protection, are handled it using airslide disintegrating mill, obtain the graphene-based conductive titanium that particle diameter is 400nm White powder.
Embodiment 6.
1）By the titanium dioxide that particle diameter is 500nm（TiO2）Add in beaker, add 100 ml deionized waters and disperseed, The solution that mass concentration is 60% is made, adds TiO2The polyethylene glycol of quality 3%, adjustment pH value of solution is 4, in 1200 W power models Interior progress ultrasound is enclosed, ultrasonic time 60min, is transferred in three-necked flask, is stirred with 600r/min.
2）Weigh 1）Middle TiO2Mass fraction is 20% graphene（It is highly conductive, suboxides group, 5~10nm of thickness, piece Footpath 500nm~20 μm）, it is added in the neopelex solution that concentration is 30%, is carried out in 1200 W power brackets Ultrasound, ultrasonic time 180min, 1 is added to by graphene solution）In, ultrasound, ultrasonic time are carried out in 300 W power brackets 24h, stirs 60min.
3）Configuration concentration is 5% cationic-type polyacrylamide（Molecular weight is 500~10,000,000）Solution, hydrolysis 60min, carries out ultrasound, polyacrylamide solution, is added drop-wise to by ultrasonic time 60min using peristaltic pump in 800W power brackets 2）In, it is added dropwise to complete in 120min, with 800 r/min, stirs 1h.
4）After reaction, it is 3 to adjust pH value, ultrasound is carried out in 600W power brackets, ultrasonic time 180min, takes out Filter, in 120 DEG C of drying, under nitrogen protection, is handled it using airslide disintegrating mill, and it is the graphene-based of 500nm to obtain particle diameter Conductive titanium dioxide.
It is to be understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this The described technical solution of inventive embodiments, it will be understood by those of ordinary skill in the art that, still the present invention can be carried out Modification or equivalent substitution, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it It is interior.

Claims (6)

  1. A kind of 1. preparation method of the graphene-based conductive titanium dioxide of high dispersive type, it is characterised in that：Implement successively as follows：
    （1）Titanium dioxide is added in beaker, deionized water is added and is disperseed, titania solution is made；Add titanium dioxide The polyglycol solution of titanium, adjustment pH value of solution are 1~4；It is ultrasonically treated；Continue and be transferred in three-necked flask, be stirred；
    （2）By step（1）The titanium dioxide of middle certain mass percentage weighs graphene；The graphene is added to dodecane In base benzene sulfonic acid sodium salt solution, it is ultrasonically treated；Graphene solution is added to step（1）In, be ultrasonically treated, continue into Row stirring；
    （3）Cationic-type polyacrylamide solution is configured, is ultrasonically treated；Polyacrylamide solution is added drop-wise to step（2） In；
    （4）After reaction, pH is adjusted, is ultrasonically treated, up to the graphene-based conductive titanium dioxide of high dispersive type.
  2. 2. the preparation method of the graphene-based conductive titanium dioxide of high dispersive type according to claim 1, it is characterised in that：Institute State step（1）In, the titanium dioxide that particle diameter is 20~500nm is added in beaker, 100ml deionized waters is added and is disperseed, The solution that mass concentration is 2%~60% is made；Add the polyglycol solution of titanium dioxide quality 0.5%~3%；400~ It is ultrasonically treated in 1200W power brackets, 10~60min of ultrasonic time, mixing speed 600r/min.
  3. 3. the preparation method of the graphene-based conductive titanium dioxide of high dispersive type according to claim 2, it is characterised in that：It is described Step（2）In, by titanium dioxide mass percent graphene is weighed for 3%~15%；The resistivity of the graphene is less than 10-3 Ω•cm；Average thickness is 5~10nm；Average piece footpath is 500nm~20 μm.
  4. 4. the preparation method of the graphene-based conductive titanium dioxide of high dispersive type according to claim 3, it is characterised in that：It is described Step（2）In, continue and be added to the graphene in the neopelex solution that mass concentration is 5%~30%, It is ultrasonically treated in 500~1200W power brackets, 30~180min of ultrasonic time；Graphene solution is added to step（1） In, it is ultrasonically treated in 100~300W power brackets, 2~24h of ultrasonic time, stirs 60min.
  5. 5. the preparation method of the graphene-based conductive titanium dioxide of high dispersive type according to claim 3 or 4, it is characterised in that： The step（3）In, configuration concentration is 0.5%~5%, molecular weight is cationic-type polyacrylamide between 500~10,000,000 Solution, hydrolyzes 10~60min；Ultrasound, 10~60min of ultrasonic time are carried out in 200~800W power brackets；Using peristaltic pump Polyacrylamide solution is added drop-wise to step（2）In, it is added dropwise to complete in 30~120min, 1h is stirred with 800 r/min speed.
  6. 6. the preparation method of the graphene-based conductive titanium dioxide of high dispersive type according to claim 5, it is characterised in that：It is described Step（4）In, after reaction, it is 1~4 to adjust pH；The progress ultrasound in 200~600W power brackets, ultrasonic time 30~ 180min, filters, and in 40~120 DEG C of drying, under nitrogen protection, it is handled using airslide disintegrating mill, obtains particle diameter as 200 The graphene-based conductive titanium dioxide of high dispersive type of~500nm.
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CN111607273A (en) * 2020-06-11 2020-09-01 北京石墨烯研究院 Graphene/titanium dioxide conductive filler and preparation method thereof
CN112375461A (en) * 2020-11-24 2021-02-19 柳州衍生科技有限公司 Conductive graphene composite coating for automobile and preparation method thereof

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CN106298283A (en) * 2016-08-24 2017-01-04 刘爽 The method manufacturing graphene-based fake capacitance type ultracapacitor

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111607273A (en) * 2020-06-11 2020-09-01 北京石墨烯研究院 Graphene/titanium dioxide conductive filler and preparation method thereof
CN112375461A (en) * 2020-11-24 2021-02-19 柳州衍生科技有限公司 Conductive graphene composite coating for automobile and preparation method thereof

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