Method for preparing hollow carbon ball with iron filler

A carbon hollow sphere, ferrocene technology, applied in the direction of coating and other directions, can solve the problems such as the absence of magnetic material in the carbon hollow sphere spherical cavity, the complex process of the carbon hollow sphere, the toxicity of raw materials, etc., and achieves low cost, high yield, good repeatability

Inactive Publication Date: 2007-05-30
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the existing problems of complex process for preparing carbon hollow spheres, high raw material toxicity, low yield, and no magnetic substance in the cavity of carbon hollow spheres, the present invention proposes a method for preparing carbon hollow spheres filled with iron to solve the problem of The concrete technical scheme of above-mentioned problem is as follows:

Method used

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Experimental program
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Effect test

specific Embodiment approach 1

[0012] Specific embodiment one, the steps of this embodiment method are as follows:

[0013] Step 1, select ferrocene and ammonium chloride as raw materials, ferrocene is 50%~80% by weight percentage, and ammonium chloride is 20%~50%;

[0014] Step 2. Mix and prepare the raw materials in step 1 evenly, put them into a polyurethane-lined grinding tank or a plastic cylinder, add ceramic balls or agate balls, and dry mix them on a ball mill for 2 to 12 hours;

[0015] Step 3. Put the uniform powder mixed and ball-milled in step 2 into a pressure reaction furnace for reaction. The protective atmosphere is argon or nitrogen. The temperature is controlled at 500-700°C, and the holding time is 0.5-4.0 hours; the by-product of the carbon hollow spheres prepared in this process is iron ammonium complex, and part of the iron ammonium complex is in the cavity of the carbon hollow sphere.

[0016] Step 4. After cooling the pressure reaction furnace in step 3 to room temperature, put the ...

specific Embodiment approach 2

[0020] Specific embodiment two, the difference between this embodiment and embodiment one is step one, get 55% ferrocene and 45% ammonium chloride by weight percentage and mix; Step two, put above-mentioned mixed material in polyurethane liner grinding tank , add agate balls as grinding balls for dry mixing, and the mixing time is 2 hours; Step 3, put the evenly mixed powder into the pressure reactor, fill it with argon to 1.9MPa, and then raise the temperature to 500°C at 30°C per minute ℃, at this time the gas pressure is 2.6MPa, heat preservation for 10 hours; step 4, after cooling with the pressure reactor, put the black powder obtained in step 3 into the tube furnace, under the argon flow of 50sccm, heat at 10 ℃ per minute Raise the temperature to 800°C and keep it warm for 4h. Other steps in this manner are the same as those in Embodiment 1.

specific Embodiment approach 3

[0021] Specific embodiment three, the difference between this embodiment and embodiment one is step one, take 66% ferrocene and 34% ammonium chloride by weight percentage and mix; Step two, put the above-mentioned mixed material in the plastic cylinder, add ceramic The balls are dry mixed, and the mixing time is 8 hours; step 3, put the mixed powder into the pressure reactor, fill it with argon to 1.9MPa, and then raise the temperature to 600°C at 20°C per minute, and the gas pressure is 2.8MPa, and keep it warm for 5 hours; step 4, after cooling with the pressure reactor, put the black powder obtained in step 3 into the tube furnace, and raise the temperature to 1050°C at 20°C per minute under an argon flow of 100sccm, and Keep warm for 2h. Other steps in this manner are the same as those in Embodiment 1.

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Abstract

The carbon hollow ball with metal filler solves the problems of existing equipment like complex process, higher poisonous material, low output, free from magnetic material inside the cavity. Picking the mixture of 50%-80% ferrocenyl and 20%-50% amchlor by weight, grinding the mixture, putting the grinded powder into air pressure reaction oven to react, putting the reacted material into tube like oven, heating to 700- 1400DEG C by argon gas and nitrogen for 1-4 hours, washing it with dilute hydrochloric acid and ionic liquid, and separating the metal filler carbon hollow ball through strong adhesion magnet. With magnetic material inside the cavity, it is simple and practical, low in cost, good in repeatability, higher in output.

Description

technical field [0001] The present invention relates to a method of preparing carbon hollow spheres with iron filling. Background technique [0002] Hollow spherical materials have many unique physical and chemical properties due to their special hollow structure. Such as lower density, better mechanical strength, large specific surface area, excellent thermal stability and permeability. And because it is point contact, it is not easy to reunite and easy to store. Therefore, it can be widely used in drug storage and transportation, artificial cells, lightweight structural materials, catalyst carriers and other fields. Among them, carbon materials have excellent biocompatibility, so carbon hollow spheres have more application potential in the field of medicine. At present, the research on carbon hollow spheres is still in its infancy, and there are only some reports on synthesis, but the process is complex, the raw materials are highly toxic, and the yield is low, which is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/18B22F9/04B22F1/02C22C1/08C01B31/02
Inventor 贾德昌刘伯洋
Owner HARBIN INST OF TECH
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