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Method for preparing carbon hollow ball with magnetic material filler

A carbon hollow sphere, magnetic material technology, applied in ferrous oxides, iron oxide/iron hydroxide and other directions, can solve the problems of high raw material toxicity, low yield, poor corrosion resistance and wear resistance, etc., to achieve excellent Biocompatibility, simple preparation process and good repeatability

Inactive Publication Date: 2007-08-29
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to solve the problems that ferric iron tetroxide nanoparticles are easy to agglomerate, have poor corrosion resistance and wear resistance during the application process, and the preparation process of hollow spheres is complicated, the raw material toxicity is high, the yield is low, and the problems are not suitable for large-scale production.

Method used

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Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0019] Specific embodiment one: the steps of this embodiment method are as follows:

[0020] Step 1, select ferrocene and ammonium chloride as raw materials, ferrocene is 50%~80% by mass percentage, ammonium chloride is 20%~50%;

[0021] 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;

[0022] 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 550-700°C, and the holding time is 0.5-4.0 hours; during this process, the iron produced by ferrocene cracking reacts with ammonium chloride to form iron ammonium complex as a liquid spherical template, and the surface adsorbs ferrocene cracking The generated carbon atoms generate carbon hollow spheres filled with ferric ammonium com...

specific Embodiment approach 2

[0026] Specific embodiment two: the steps of this embodiment method are as follows:

[0027] Step 1, select ferrocene and ammonium chloride as raw materials, ferrocene is 50%~80% by mass percentage, ammonium chloride is 20%~50%;

[0028] 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;

[0029] 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 550-700°C, and the holding time is 0.5-4.0 hours; during this process, the iron produced by ferrocene cracking reacts with ammonium chloride to form iron ammonium complex as a liquid spherical template, and the surface adsorbs ferrocene cracking The generated carbon atoms generate carbon hollow spheres filled with ferric ammonium com...

specific Embodiment approach 3

[0033] Specific embodiment three: the difference between this embodiment and embodiment one is that step one, ferrocene and ammonium chloride are mixed by mass ratio 4: 3, a total of 70 grams, step two, put in polyurethane lining grinding tank Or in a plastic cylinder, add ceramic balls or agate balls as grinding balls for dry mixing, the mixing time is 2 hours; step 3, put the evenly mixed powder directly in the pressure furnace, fill it with argon to 1.9MPa, and then Raise the temperature at a rate of 30°C to 550°C, at this time the gas pressure is 2.6MPa, and keep warm for 4 hours; cool with the furnace, step 4, put the obtained black powder into deionized water under air atmosphere and stir for 1 hour; step 5, Put the black powder obtained after the hydrolysis treatment in a tube furnace, raise the temperature to 500° C. at a rate of 10° C. per minute under an argon flow of 50 sccm, and keep it warm for 1 hour; step 6, put the black powder obtained after the heat treatment ...

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Abstract

The invention relates to a manufacturing method for carbon hollow ball filed by magnetic material. It includes the following steps: mixing ferrocene 50-80wt% with ammonium chloride 20-50wt%, taking ball milling to the raw material; putting into pressure reacting furnace to take reaction; the reacted black powder would be put into deionized water to take hydrolysis after cooling; taking thermal process in tubular furnace to the product after reacting; putting the product into Buchner filter, taking washing and filtering by thick hydrochloric acid to gain carbon hollow ball containing magnetic material. The invention has the advantages of low cost, good repeatability, and high yield.

Description

technical field [0001] The invention relates to a preparation method of carbon hollow spheres. Background technique [0002] Hollow spherical materials have many unique physical and chemical properties due to their special hollow structure: such as low density, certain mechanical strength, large specific surface area, excellent thermal stability, permeability, etc.; and because of point contact , so it is not easy to reunite and easy to store. Therefore, it can be widely used in the fields of drug storage and transportation, artificial cells, lightweight structural materials, damping materials, and catalyst carriers. Among them, carbon hollow spheres have excellent biocompatibility, and are easy to modify the surface, so that the surface has other functional groups, so carbon hollow spheres have more application potential in the field of medicine. Ferroferric oxide has been widely used in scientific research and commercial fields due to its magnetic responsiveness. Moreov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01G49/08
Inventor 贾德昌刘伯洋周玉
Owner HARBIN INST OF TECH