CN103265006A - Preparation method of titanium dioxide evenly-loaded carbon nanorod - Google Patents
Preparation method of titanium dioxide evenly-loaded carbon nanorod Download PDFInfo
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- CN103265006A CN103265006A CN2013101766846A CN201310176684A CN103265006A CN 103265006 A CN103265006 A CN 103265006A CN 2013101766846 A CN2013101766846 A CN 2013101766846A CN 201310176684 A CN201310176684 A CN 201310176684A CN 103265006 A CN103265006 A CN 103265006A
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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
Technical field
The present invention relates to a kind of is carrier with the carbon nano rod, and the titanium dioxide uniform loading belongs to field of nanometer technology in the preparation method of its surperficial composite carbon nanometer rod.
Background technology
TiO
2Physicochemical property stable, has good photoelectric property, nontoxic to Biosafety, the source is abundant, and thereby the light induced electron that produces-hole electromotive force current potential height has very strong oxidisability and 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 big, pore structure and surface chemical property are controlled, surface key attitude is different with granule interior with electronic state, the not congruent defective locations on surface that causes of surface atom coordination increases, possessed the good condition as support of the catalyst, therefore, be applied to catalytic field more and more widely in recent years.
Summary of the invention
The objective 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 objective of the invention is to finish by following technical solution, it selects titanate nanotube for use 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) with titanyl sulfate (TiOSO
4), L-Methionin, and sodium lauryl sulphate is after the ratio of 100-130:15-40:1-5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 40-60ml ultrapure water with the ratio of mass ratio 10-30:1-15 with this powdered mixture and titanate nanotube, stirred 40-60 minute, and put into hydrothermal reaction kettle and react;
3) after reacting 2-5 hour under the 160-180 ℃ of temperature, naturally cooling 6-10 hour; With the centrifugal 5-10 of reactant minute, dehydrated alcohol cleaned 2-4 time afterwards, descended dry 8-12 hour at 60-80 ℃, namely got target product after the grinding.
Optimized technical scheme of the present invention is: 1) with TiOSO
4, L-Methionin, and sodium lauryl sulphate is after the ratio of 115:25:3 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 50ml ultrapure water with the ratio of mass ratio 20:8 with this powdered mixture and titanate nanotube, stirred 50 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 3.5 hours under 170 ℃ of temperature, naturally cooling 8 hours; With centrifugal 7 minutes of reactant, dehydrated alcohol cleaned 3 times afterwards, 70 ℃ dry 10 hours down, namely get target product after the grinding.
Titanate nanotube of the present invention is that the carbon nano rod of skeleton is made as follows:
1) with starch, L-Methionin, and sodium lauryl sulphate is after the ratio of 100-150:7-20:1-5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the titanate nanotube of 4-10nm joins in the 40-60ml ultrapure water with the ratio of mass ratio 10-20:1-10 with this powdered mixture and homemade caliber, ultrasonic 5-15 minute, and put into hydrothermal reaction kettle and react;
3) after reacting 5-9 hours under the 160-180 ℃ of temperature, naturally cooling 6-10 hour; With the centrifugal 5-10 of reactant minute, dehydrated alcohol cleaned 2-4 time afterwards, descended dry 8-12 hour at 60-80 ℃, namely got target product after the grinding.
Beneficial effect of the present invention: preparation condition gentleness of the present invention, method is simple, and is workable, and repeatability is better, and cost is lower, has certain universality.
Description of 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
The present invention will be described in detail below in conjunction with drawings and Examples: the present invention is that to select titanate nanotube for use 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) with TiOSO
4, L-Methionin, and sodium lauryl sulphate is after the ratio of 100-130:15-40:1-5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 40-60ml ultrapure water with the ratio of mass ratio 10-30:1-15 with this powdered mixture and titanate nanotube, stirred 40-60 minute, and put into hydrothermal reaction kettle and react;
3) after reacting 2-5 hour under the 160-180 ℃ of temperature, naturally cooling 6-10 hour; With the centrifugal 5-10 of reactant minute, dehydrated alcohol cleaned 2-4 time afterwards, descended dry 8-12 hour at 60-80 ℃, namely got target product after the grinding.
Embodiment 1: preparation method of the present invention comprises the steps:
1) with TiOSO
4, L-Methionin, and sodium lauryl sulphate is after the ratio of 115:25:3 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 50ml ultrapure water with the ratio of mass ratio 20:8 with this powdered mixture and titanate nanotube, stirred 50 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 3.5 hours under 170 ℃ of temperature, naturally cooling 8 hours; With centrifugal 7 minutes of reactant, dehydrated alcohol cleaned 3 times afterwards, 70 ℃ dry 10 hours down, namely get target product after the grinding.
Embodiment 2: preparation method of the present invention comprises the steps:
1) with TiOSO
4, L-Methionin, and sodium lauryl sulphate is after the ratio of 100:15:1 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 40ml ultrapure water with the ratio of mass ratio 10:1 with this powdered mixture and titanate nanotube, stirred 40 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 2 hours under 160 ℃ of temperature, naturally cooling 6 hours; With centrifugal 5 minutes of reactant, dehydrated alcohol cleaned 2 times afterwards, 60 ℃ dry 8 hours down, namely get target product after the grinding.
Embodiment 3: preparation method of the present invention comprises the steps:
1) with TiOSO
4, L-Methionin, and sodium lauryl sulphate is after the ratio of 130:40:5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 60ml ultrapure water with the ratio of mass ratio 30:15 with this powdered mixture and titanate nanotube, stirred 60 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 5 hours under 180 ℃ of temperature, naturally cooling 10 hours; With centrifugal 10 minutes of reactant, dehydrated alcohol cleaned 4 times afterwards, 80 ℃ dry 12 hours down, namely get target product after the grinding.
Embodiment 4: preparation method of the present invention comprises the steps:
1) with TiOSO
4, L-Methionin, and sodium lauryl sulphate is after the ratio of 100:20:2 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 40ml ultrapure water with the ratio of mass ratio 10:7 with this powdered mixture and titanate nanotube, stirred 40 minutes, and put into hydrothermal reaction kettle and react;
3) 160 ℃ are reacted after 2 hours naturally cooling 8 hours; With centrifugal 5 minutes of reactant, dehydrated alcohol cleaned 3 times afterwards, 80 ℃ dry 12 hours down, namely get target product after the grinding.
Shown in Figure 1 is the transmission electron microscope picture of titanium dioxide equally loaded carbon nano rod; Shown in Figure 2 is the high power transmission electron microscope picture of titanium dioxide equally loaded carbon nano rod; The 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 technique known preparation for use, also can make by being prepared as follows method, and described preparation method is:
1) with starch, L-Methionin, and sodium lauryl sulphate is after the ratio of 100-150:7-20:1-5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the titanate nanotube of 4-10nm joins in the 40-60ml ultrapure water with the ratio of mass ratio 10-20:1-10 with this powdered mixture and homemade caliber, ultrasonic 5-15 minute, and put into hydrothermal reaction kettle and react;
3) after reacting 5-9 hours under the 160-180 ℃ of temperature, naturally cooling 6-10 hour; With the centrifugal 5-10 of reactant minute, dehydrated alcohol cleaned 2-4 time afterwards, descended dry 8-12 hour at 60-80 ℃, namely got the carbon nano rod that titanate nanotube is skeleton after the grinding.
The described titanate nanotube of concrete preparation is that the carbon nano rod method of skeleton has:
Embodiment 5: titanate nanotube of the present invention is that the preparation method of the carbon nano rod of skeleton comprises following several steps:
1) with starch, L-Methionin, and sodium lauryl sulphate is after the ratio of 120:10:3 fully mixes with the mass ratio, forms powdered mixture;
2) be that the titanate nanotube of 6-8nm joins in the 50ml ultrapure water with the ratio of mass ratio 15:5 with this powdered mixture and homemade caliber, ultrasonic 10 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 7 hours under 170 ℃ of temperature, naturally cooling 8 hours; With centrifugal 8 minutes of reactant, dehydrated alcohol cleaned 3 times afterwards, 70 ℃ dry 10 hours down, namely get the carbon nano rod that titanate nanotube is skeleton after the grinding.
Embodiment 6: titanate nanotube of the present invention is that the preparation method of the carbon nano rod of skeleton comprises following several steps:
1) with starch, L-Methionin, and sodium lauryl sulphate is after the ratio of 100:15:3 fully mixes with the mass ratio, forms powdered mixture;
2) be that the titanate nanotube of 5nm joins in the 40ml ultrapure water with the ratio of mass ratio 15:3 with this mixture and homemade caliber, ultrasonic 5 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 7 hours under 180 ℃ of temperature, naturally cooling 8 hours; With centrifugal 5 minutes of reactant, dehydrated alcohol cleaned 3 times afterwards, 80 ℃ dry 8 hours down, namely get the carbon nano rod that titanate nanotube is skeleton after the grinding.
Embodiment 7, and titanate nanotube of the present invention is that the preparation method of the carbon nano rod of skeleton comprises following several steps:
1) with starch, L-Methionin, and sodium lauryl sulphate is after the ratio of 100:7:1 fully mixes with the mass ratio, forms powdered mixture;
2) be that the titanate nanotube of 4nm joins in the 40ml ultrapure water with the ratio of mass ratio 10:1 with this powdered mixture and homemade caliber, ultrasonic 5 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 5 hours under 160 ℃ of temperature, naturally cooling 6 hours; With centrifugal 5 minutes of reactant, dehydrated alcohol cleaned 2 times afterwards, 60 ℃ dry 8 hours down, namely get the carbon nano rod that titanate nanotube is skeleton after the grinding.
Embodiment 8, and titanate nanotube of the present invention is that the preparation method of the carbon nano rod of skeleton comprises following several steps:
1) with starch, L-Methionin, and sodium lauryl sulphate is after the ratio of 150:20:5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the titanate nanotube of 10nm joins in the 60ml ultrapure water with the ratio of mass ratio 20:10 with this powdered mixture and homemade caliber, ultrasonic 15 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 9 hours under 180 ℃ of temperature, naturally cooling 10 hours; With centrifugal 10 minutes of reactant, dehydrated alcohol cleaned 4 times afterwards, 80 ℃ dry 12 hours down, namely get the carbon nano rod that titanate nanotube is skeleton after the grinding.
Following examples only are 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 enforceable numerous embodiment easily.
Claims (3)
1. the preparation method of a titanium dioxide equally loaded carbon nano rod is characterized in that it selects titanate nanotube for use 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) with titanyl sulfate (TiOSO
4), L-Methionin, and sodium lauryl sulphate is after the ratio of 100-130:15-40:1-5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 40-60ml ultrapure water with the ratio of mass ratio 10-30:1-15 with this powdered mixture and titanate nanotube, stirred 40-60 minute, and put into hydrothermal reaction kettle and react;
3) after reacting 2-5 hour under the 160-180 ℃ of temperature, naturally cooling 6-10 hour; With the centrifugal 5-10 of reactant minute, dehydrated alcohol cleaned 2-4 time afterwards, descended dry 8-12 hour at 60-80 ℃, namely got target product after the grinding.
2. the preparation method of titanium dioxide equally loaded carbon nano rod according to claim 1 is characterized in that in this preparation method's the step:
1) with TiOSO
4, L-Methionin, and sodium lauryl sulphate is after the ratio of 115:25:3 fully mixes with the mass ratio, forms powdered mixture;
2) be that the carbon nano rod of skeleton joins in the 50ml ultrapure water with the ratio of mass ratio 20:8 with this powdered mixture and titanate nanotube, stirred 50 minutes, and put into hydrothermal reaction kettle and react;
3) after reacting 3.5 hours under 170 ℃ of temperature, naturally cooling 8 hours; With centrifugal 7 minutes of reactant, dehydrated alcohol cleaned 3 times afterwards, 70 ℃ dry 10 hours down, namely get target product after the grinding.
3. the preparation method of titanium dioxide equally loaded carbon nano rod according to claim 1 is characterized in that described titanate nanotube is that the carbon nano rod of skeleton is made as follows:
1) with starch, L-Methionin, and sodium lauryl sulphate is after the ratio of 100-150:7-20:1-5 fully mixes with the mass ratio, forms powdered mixture;
2) be that the titanate nanotube of 4-10nm joins in the 40-60ml ultrapure water with the ratio of mass ratio 10-20:1-10 with this powdered mixture and homemade caliber, ultrasonic 5-15 minute, and put into hydrothermal reaction kettle and react;
3) after reacting 5-9 hours under the 160-180 ℃ of temperature, naturally cooling 6-10 hour; With the centrifugal 5-10 of reactant minute, dehydrated alcohol cleaned 2-4 time afterwards, descended dry 8-12 hour at 60-80 ℃, namely got the carbon nano rod that titanate nanotube is skeleton after the grinding.
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| CN108704634A (en) * | 2018-05-11 | 2018-10-26 | 南昌航空大学 | A kind of TiO2TiO is loaded on nano wire2The preparation method of the photochemical catalyst of nano particle |
Citations (3)
| 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 |
| US20110157772A1 (en) * | 2009-12-28 | 2011-06-30 | Aruna Zhamu | Spacer-modified nano graphene electrodes for supercapacitors |
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Patent Citations (3)
| 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 |
| US20110157772A1 (en) * | 2009-12-28 | 2011-06-30 | Aruna Zhamu | Spacer-modified nano graphene electrodes for supercapacitors |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108704634A (en) * | 2018-05-11 | 2018-10-26 | 南昌航空大学 | A kind of TiO2TiO is loaded on nano wire2The preparation method of the photochemical catalyst of nano particle |
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