CN103265006B - Preparation method of titanium dioxide evenly-loaded carbon nanorod - Google Patents

Preparation method of titanium dioxide evenly-loaded carbon nanorod Download PDF

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CN103265006B
CN103265006B CN201310176684.6A CN201310176684A CN103265006B CN 103265006 B CN103265006 B CN 103265006B CN 201310176684 A CN201310176684 A CN 201310176684A CN 103265006 B CN103265006 B CN 103265006B
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carbon nano
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CN103265006A (en
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王晟
王騊
徐友峰
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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Abstract

The invention relates to a preparation method of a titanium dioxide evenly-loaded carbon nanorod. According to the preparation method, the titanium dioxide evenly-loaded carbon nanorod composite material is finally obtained by using a carbon nanorod taking a titanate nanotube as the skeleton as a carrier and loading TiO2 nanoparticles through a hydrothermal method. The preparation method comprises the following specific steps: 1) thoroughly and evenly mixing titanyl sulfate (TiOSO4), L-lysine and sodium lauryl sulfate according to a mass ratio of (100-130):(15-40):(1-5) to form a powder mixture; 2) adding the powder mixture and the carbon nanorod taking a titanate nanotube as the skeleton into 40-60ml of ultrapure water according to a mass ratio of (10-30):(1-15), stirring for 40-60 minutes, and reacting in a hydrothermal reaction kettle; and 3) reacting at 160-180 DEG C for 2-5 hours, naturally cooling for 6-10 hours, centrifuging the reaction product for 5-10 minutes, cleaning with anhydrous ethanol 2-4 times, drying at 60-80 DEG C for 8-12 hours, and grinding to obtain the target product. The preparation method has the characteristics of mild preparation conditions, simple and easy method, high operability, satisfactory repetitiveness, low cost, certain universality and the like.

Description

A kind of preparation method of titanium dioxide equally loaded carbon nano rod
Technical field
The present invention relates to one taking carbon nano rod as carrier, titanium dioxide uniform loading, in the preparation method of its surperficial composite carbon nanometer rod, belongs to field of nanometer technology.
Background technology
TiO 2physicochemical property stable, there is good photoelectric property, nontoxic to Biosafety, source is abundant, and thereby the light induced electron-hole electromotive force current potential producing is high has very strong oxidisability and a reductibility, be a kind of good photocatalyst, and be acknowledged as the environment-friendly type photocatalyst material of the tool development and application potentiality in environment pollution treatment field.
Carbon nano rod is because size is little, specific surface area is large, pore structure and surface chemical property are controlled, surface key state is different from granule interior with electronic state, surface atom coordination is not congruent causes surperficial defective locations to increase, possess the good condition as support of the catalyst, therefore, be applied to more and more widely catalytic field in recent years.
Summary of the invention
The object of the invention is to overcome the deficiency that prior art exists, and provide a kind of method simple, workable, repeatability is better, the preparation method of lower-cost titanium dioxide equally loaded carbon nano rod.
The object of the invention is to complete by following technical solution, it selects titanate nanotube is that the carbon nano rod of skeleton is carrier, by hydrothermal method load TiO 2nano particle, finally obtains a kind of titanium dioxide equally loaded carbon nano rod matrix material, and concrete step is:
1) by titanyl sulfate (TiOSO 4), 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100-130:15-40:1-5 fully mix, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 40-60ml ultrapure water with the ratio of mass ratio 10-30:1-15, stirs 40-60 minute, and puts into hydrothermal reaction kettle and react;
3) at 160-180 DEG C of temperature, react after 2-5 hour naturally cooling 6-10 hour; By centrifugal reactant 5-10 minute, dehydrated alcohol cleans 2-4 time afterwards, and at 60-80 DEG C, dry 8-12 hour, obtains target product after grinding.
The preferred technical scheme of the present invention is: 1) by TiOSO 4, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 115:25:3 fully mix, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 50ml ultrapure water with the ratio of mass ratio 20:8, stirs 50 minutes, and puts into hydrothermal reaction kettle and react;
3) at 170 DEG C of temperature, react after 3.5 hours naturally cooling 8 hours; By centrifugal reactant 7 minutes, dehydrated alcohol cleaned 3 times afterwards, at 70 DEG C, was dried 10 hours, obtained target product after grinding.
Titanate nanotube of the present invention is that the carbon nano rod of skeleton is made as follows:
1) by starch, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100-150:7-20:1-5 fully mix, form powdered mixture;
2) titanate nanotube that is 4-10nm by this powdered mixture and homemade caliber joins in 40-60ml ultrapure water with the ratio of mass ratio 10-20:1-10, ultrasonic 5-15 minute, and put into hydrothermal reaction kettle and react;
3) at 160-180 DEG C of temperature, react after 5-9 hours naturally cooling 6-10 hour; By centrifugal reactant 5-10 minute, dehydrated alcohol cleans 2-4 time afterwards, and at 60-80 DEG C, dry 8-12 hour, obtains target product after grinding.
Beneficial effect of the present invention: preparation condition gentleness of the present invention, method is simple, workable, and better, cost is lower, has certain universality for repeatability.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of titanium dioxide equally loaded carbon nano rod of the present invention.
Fig. 2 is the high power transmission electron microscope picture of titanium dioxide equally loaded carbon nano rod of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described in detail: the present invention is that to select titanate nanotube be that the carbon nano rod of skeleton is carrier, by hydrothermal method load TiO 2nano particle, finally obtains a kind of titanium dioxide equally loaded carbon nano rod matrix material, and concrete step is:
1) by TiOSO 4, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100-130:15-40:1-5 fully mix, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 40-60ml ultrapure water with the ratio of mass ratio 10-30:1-15, stirs 40-60 minute, and puts into hydrothermal reaction kettle and react;
3) at 160-180 DEG C of temperature, react after 2-5 hour naturally cooling 6-10 hour; By centrifugal reactant 5-10 minute, dehydrated alcohol cleans 2-4 time afterwards, and at 60-80 DEG C, dry 8-12 hour, obtains target product after grinding.
Embodiment 1: preparation method of the present invention comprises the steps:
1) by TiOSO 4, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 115:25:3 fully mix, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 50ml ultrapure water with the ratio of mass ratio 20:8, stirs 50 minutes, and puts into hydrothermal reaction kettle and react;
3) at 170 DEG C of temperature, react after 3.5 hours naturally cooling 8 hours; By centrifugal reactant 7 minutes, dehydrated alcohol cleaned 3 times afterwards, at 70 DEG C, was dried 10 hours, obtained target product after grinding.
Embodiment 2: preparation method of the present invention comprises the steps:
1) by TiOSO 4, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100:15:1 fully mix, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 40ml ultrapure water with the ratio of mass ratio 10:1, stirs 40 minutes, and puts into hydrothermal reaction kettle and react;
3) at 160 DEG C of temperature, react after 2 hours naturally cooling 6 hours; By centrifugal reactant 5 minutes, dehydrated alcohol cleaned 2 times afterwards, at 60 DEG C, was dried 8 hours, obtained target product after grinding.
Embodiment 3: preparation method of the present invention comprises the steps:
1) by TiOSO 4, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 130:40:5 fully mix, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 60ml ultrapure water with the ratio of mass ratio 30:15, stirs 60 minutes, and puts into hydrothermal reaction kettle and react;
3) at 180 DEG C of temperature, react after 5 hours naturally cooling 10 hours; By centrifugal reactant 10 minutes, dehydrated alcohol cleaned 4 times afterwards, at 80 DEG C, was dried 12 hours, obtained target product after grinding.
Embodiment 4: preparation method of the present invention comprises the steps:
1) by TiOSO 4, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100:20:2 fully mix, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 40ml ultrapure water with the ratio of mass ratio 10:7, stirs 40 minutes, and puts into hydrothermal reaction kettle and react;
3) 160 DEG C were reacted after 2 hours, naturally cooling 8 hours; By centrifugal reactant 5 minutes, dehydrated alcohol cleaned 3 times afterwards, at 80 DEG C, was dried 12 hours, obtained target product after grinding.
Shown in Fig. 1 is the transmission electron microscope picture of titanium dioxide equally loaded carbon nano rod; Shown in Fig. 2 is the high power transmission electron microscope picture of titanium dioxide equally loaded carbon nano rod; Surface is for having the TiO 2 particles of lattice line.
Titanate nanotube of the present invention is that the carbon nano rod of skeleton can be selected existing known technology preparation, also can make by being prepared as follows method, and described preparation method is:
1) by starch, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100-150:7-20:1-5 fully mix, form powdered mixture;
2) titanate nanotube that is 4-10nm by this powdered mixture and homemade caliber joins in 40-60ml ultrapure water with the ratio of mass ratio 10-20:1-10, ultrasonic 5-15 minute, and put into hydrothermal reaction kettle and react;
3) at 160-180 DEG C of temperature, react after 5-9 hours naturally cooling 6-10 hour; By centrifugal reactant 5-10 minute, dehydrated alcohol cleans 2-4 time afterwards, and at 60-80 DEG C, dry 8-12 hour, obtains the carbon nano rod that titanate nanotube is skeleton after grinding.
The carbon nano rod method that the described titanate nanotube of concrete preparation is skeleton has:
Embodiment 5: the preparation method of the carbon nano rod that titanate nanotube of the present invention is skeleton comprises following several step:
1) by starch, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 120:10:3 fully mix, form powdered mixture;
2) titanate nanotube that is 6-8nm by this powdered mixture and homemade caliber joins in 50ml ultrapure water with the ratio of mass ratio 15:5, and ultrasonic 10 minutes, and put into hydrothermal reaction kettle and react;
3) at 170 DEG C of temperature, react after 7 hours naturally cooling 8 hours; By centrifugal reactant 8 minutes, dehydrated alcohol cleaned 3 times afterwards, at 70 DEG C, was dried 10 hours, obtained the carbon nano rod that titanate nanotube is skeleton after grinding.
Embodiment 6: the preparation method of the carbon nano rod that titanate nanotube of the present invention is skeleton comprises following several step:
1) by starch, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100:15:3 fully mix, form powdered mixture;
2) titanate nanotube that is 5nm by this mixture and homemade caliber joins in 40ml ultrapure water with the ratio of mass ratio 15:3, and ultrasonic 5 minutes, and put into hydrothermal reaction kettle and react;
3) at 180 DEG C of temperature, react after 7 hours naturally cooling 8 hours; By centrifugal reactant 5 minutes, dehydrated alcohol cleaned 3 times afterwards, at 80 DEG C, was dried 8 hours, obtained the carbon nano rod that titanate nanotube is skeleton after grinding.
Embodiment 7, the preparation method of the carbon nano rod that titanate nanotube of the present invention is skeleton comprises following several step:
1) by starch, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 100:7:1 fully mix, form powdered mixture;
2) titanate nanotube that is 4nm by this powdered mixture and homemade caliber joins in 40ml ultrapure water with the ratio of mass ratio 10:1, and ultrasonic 5 minutes, and put into hydrothermal reaction kettle and react;
3) at 160 DEG C of temperature, react after 5 hours naturally cooling 6 hours; By centrifugal reactant 5 minutes, dehydrated alcohol cleaned 2 times afterwards, at 60 DEG C, was dried 8 hours, obtained the carbon nano rod that titanate nanotube is skeleton after grinding.
Embodiment 8, the preparation method of the carbon nano rod that titanate nanotube of the present invention is skeleton comprises following several step:
1) by starch, 1B, and after the ratio of sodium lauryl sulphate taking mass ratio as 150:20:5 fully mix, form powdered mixture;
2) titanate nanotube that is 10nm by this powdered mixture and homemade caliber joins in 60ml ultrapure water with the ratio of mass ratio 20:10, and ultrasonic 15 minutes, and put into hydrothermal reaction kettle and react;
3) at 180 DEG C of temperature, react after 9 hours naturally cooling 10 hours; By centrifugal reactant 10 minutes, dehydrated alcohol cleaned 4 times afterwards, at 80 DEG C, was dried 12 hours, obtained the carbon nano rod that titanate nanotube is skeleton after grinding.
Following examples are only the several specific embodiments of the present invention, and on the basis of above-mentioned public technology scheme, those skilled in the art can replace by simple numerical value, can obtain easily enforceable numerous embodiment.

Claims (2)

1. the preparation method of a titanium dioxide equally loaded carbon nano rod, it is characterized in that it selects titanate nanotube is that the carbon nano rod of skeleton is carrier, by hydrothermal method load TiO2 nano particle, finally obtain a kind of titanium dioxide equally loaded carbon nano rod matrix material, concrete step is:
1) by titanyl sulfate (TiOSO4), L-Methionin, and sodium lauryl sulphate is taking mass ratio as 100-130: after the ratio of 15-40: 1-5 fully mixes, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 40-60ml ultrapure water with the ratio of mass ratio 10-30: 1-15, stirs 40-60 minute, and puts into hydrothermal reaction kettle and react;
3) at 160-180 DEG C of temperature, react after 2-5 hour naturally cooling 6-10 hour; By centrifugal reactant 5-10 minute, dehydrated alcohol cleans 2-4 time afterwards, and at 60-80 DEG C, dry 8-12 hour, obtains target product after grinding;
Described titanate nanotube is that the carbon nano rod of skeleton is made as follows:
1) by starch, L-Methionin, and sodium lauryl sulphate is taking mass ratio as 100-150: after the ratio of 7-20: 1-5 fully mixes, form powdered mixture;
2) titanate nanotube that is 4-10nm by this powdered mixture and homemade caliber joins in 40-60ml ultrapure water with the ratio of mass ratio 10-20: 1-10, ultrasonic 5-15 minute, and put into hydrothermal reaction kettle and react;
3) at 160-180 DEG C of temperature, react after 5-9 hours naturally cooling 6-10 hour; By centrifugal reactant 5-10 minute, dehydrated alcohol cleans 2-4 time afterwards, and at 60-80 DEG C, dry 8-12 hour, obtains the carbon nano rod that titanate nanotube is skeleton after grinding.
2. according to the preparation method of the titanium dioxide equally loaded carbon nano rod described in claim 1, it is characterized in that in this preparation method's step:
1) by TiOSO4, L-Methionin, and sodium lauryl sulphate taking mass ratio after the ratio of 115: 25: 3 fully mixes, form powdered mixture;
2) carbon nano rod that is skeleton by this powdered mixture and titanate nanotube joins in 50ml ultrapure water with the mass ratio ratio of 20: 8, stirs 50 minutes, and puts into hydrothermal reaction kettle and react;
3) at 170 DEG C of temperature, react after 3.5 hours naturally cooling 8 hours; By centrifugal reactant 7 minutes, dehydrated alcohol cleaned 3 times afterwards, at 70 DEG C, was dried 10 hours, obtained target product after grinding.
CN201310176684.6A 2013-05-13 2013-05-13 Preparation method of titanium dioxide evenly-loaded carbon nanorod Expired - Fee Related CN103265006B (en)

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Citations (2)

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Publication number Priority date Publication date Assignee Title
CN1868589A (en) * 2006-06-22 2006-11-29 厦门大学 Method for preparing carbon nanometer tube/titanium dioxide composite photocatalyst
CN101318646A (en) * 2008-07-11 2008-12-10 浙江大学 Method for preparing TiO2 coated carbon nano-tube composite material

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US8315039B2 (en) * 2009-12-28 2012-11-20 Nanotek Instruments, Inc. Spacer-modified nano graphene electrodes for supercapacitors

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1868589A (en) * 2006-06-22 2006-11-29 厦门大学 Method for preparing carbon nanometer tube/titanium dioxide composite photocatalyst
CN101318646A (en) * 2008-07-11 2008-12-10 浙江大学 Method for preparing TiO2 coated carbon nano-tube composite material

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