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Transition metal oxide/silicon dioxide nano composite powder body catalyst, its synthesis method and carbon nano tube prepared by using said catalyst

A nano-composite powder, transition metal technology, applied in metal/metal oxide/metal hydroxide catalysts, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve the problem of wide distribution, non-uniformity, particle size Large and other problems, to achieve the effect of less equipment investment, simple process and low cost

Inactive Publication Date: 2003-03-05
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of carbon nanotubes by catalytic cracking usually requires the use of transition metals (Ni, Co, Fe) or their compounds as catalysts. The effective dispersion and size of catalyst particles are one of the key factors for the synthesis of carbon nanotubes. Currently, the commonly used sol - The catalyst powder synthesized by the gel atmospheric pressure drying method has poor dispersibility, large and uneven particle size, and the resulting carbon nanotubes have a low yield, large diameter, and wide distribution range, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1. Synthetic catalyst

[0019] (1) Ethyl orthosilicate and nickel nitrate aqueous solution are mixed at room temperature with a molar ratio of silicon: nickel of 1:8, stirred for 12 hours, slowly dripped with dilute ammonia water (nickel, ammonia molar ratio is 1:6), and then Stir and stand for 12 hours each, then wash and filter with suction to obtain a binary colloid precursor.

[0020] (2) After the binary colloid is washed and filtered, it is placed in an autoclave, and deionized water is added, and the filling degree of the still cavity is 60%, and then the temperature is raised to 200 degrees Celsius at a rate of 80 degrees Celsius / hour, and the temperature is kept for 3 hours to obtain NiO 2 / SiO 2 Composite powder catalyst.

[0021] 2. Preparation of carbon nanotubes

[0022] Get 100 milligrams of catalysts, heat up to 550 degrees centigrade under a nitrogen atmosphere, pass hydrogen for reduction for 0.5 hours, feed reaction gas (acetylene: hydrogen=2:1) ​​a...

Embodiment 2

[0024] Same as other conditions and steps of Example 1, change the mixed solution silicon, nickel molar ratio is 1: 12, nickel, ammonia molar ratio is 1: 9, the filling degree of the medium in the kettle is 70%, and the hydrothermal reaction temperature is 230 degrees centigrade, Preparation of NiO / SiO 2 Composite powder catalyst.

[0025] The obtained product (catalyst has been subtracted) is 210 mg, containing more than 90% of carbon nanotubes (that is, little amorphous carbon is formed), and the tube diameter is 10-23 nanometers, most of which are 20 nanometers.

Embodiment 3

[0027] Same as other conditions and steps in Example 2, change silicon, nickel molar ratio to 1: 14, obtain product ((catalyst has been subtracted)) 170 mg, containing more than 85% of carbon nanotubes, tube diameter 10-30 nanometers, most is 25 nm.

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Abstract

The present invention relates to a method for synthesizing transition metal oxide / silicon dioxide nano composite powder catalyst. Said invention adopts precursor hydrothermal method to make synthesis, and said catalyst can be used for preparing carbon nano tube, and said method includes the following steps: placing the catalyst into the catalytic bed quartz tube, heating to 500-600 deg.C under the condition of inert gas atmosphere, introducing hydrogen gas and reducing for 0.4-1.5 hr, when the temp. is reached to 630-780 deg.C, introducing acetylene and hydrogen gas whose volume ratio is 9:1-1:1 in the flowing rate of 40-200 ml / min to make it prduce cracking reaction to synthesize carbon nano tube, its reaction time is 0.5-1.0 hr.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and more specifically relates to a transition metal oxide / silicon dioxide nanocomposite powder catalyst and a synthesis method thereof, as well as a method for the catalyst to prepare carbon nanotubes. Background technique [0002] Carbon nanotubes have been recognized internationally as a new type of functional material and structural material with excellent performance, which can be used as high-density hydrogen storage materials, high-strength composite materials, high-definition flat panel displays, nano-devices and new electromagnetic wave-absorbing materials Wait. At present, there are mainly three methods for preparing carbon nanotubes: catalytic cracking method, arc method and laser evaporation method. The preparation of carbon nanotubes by catalytic cracking usually requires the use of transition metals (Ni, Co, Fe) or their compounds as catalysts. The effective dispers...

Claims

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Application Information

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IPC IPC(8): B01J23/08B01J23/74B01J37/03C01B31/02
Inventor 朱燕娟邓淑华张海燕陈易明何艳阳陈玉莲
Owner GUANGDONG UNIV OF TECH
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