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Micro carbon roll, process for preparing same and use thereof

A micro-carbon, carbon source gas technology, applied in textiles and papermaking, fiber chemical characteristics, etc., can solve the problems of cumbersome operation process, environmental pollution, unfavorable industrial production, etc., achieves low degree of graphitization, enhanced mechanical properties, and broad application Foreground effect

Inactive Publication Date: 2007-07-25
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, one of the defects of this method is that impurities containing sulfur or phosphorus need to be continuously introduced during the preparation process, which makes the exhaust tail gas also contain a certain amount of sulfur or phosphorus, thereby polluting the environment.
In addition, it is disclosed in the specific embodiment of the patent notification number CN1098941C that in order to obtain a regular and uniform product, the synthesis conditions must be strictly controlled, and the substrate on which the catalyst is placed must be moved downward as the fiber grows. These requirements are for industrial production. It is said to be difficult to achieve; the technical solution disclosed by the patent announcement number CN1120252C is to control the reaction process through a complex set of devices, and the operation process is very complicated, which is also unfavorable for realizing industrial production; the technology disclosed by the patent announcement number CN1113990C The implementation process of the scheme is relatively simple and convenient, but the shape of the micro carbon coils obtained by this method is irregular, and the product is not uniform
[0004] After analysis, it is found that the existing technology for preparing helical carbon fibers (i.e. micro-carbon rolls) mainly has the following two deficiencies: (1) producing sulfur-containing or phosphorus-containing tail gas, which pollutes the environment; (2) preparation efficiency, product The morphology is sensitive to the synthesis conditions, and the synthesis conditions must be strictly controlled, which is not conducive to the realization of industrial production

Method used

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  • Micro carbon roll, process for preparing same and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Mix 5.8g of nickel powder (5μm) and 3.5g of sulfur powder evenly, place it in a porcelain boat, and place it in a horizontally placed quartz reaction tube (40×1200mm), heat it to 600°C under nitrogen protection and keep it for 1 hour. After cooling and grinding, a nickel sulfide catalyst was obtained, the mass percent content: nickel 73.3%, sulfur 26.7%.

Embodiment 2

[0021] Take 6.0g of cobalt-nickel alloy powder (0.5μm) and 2.3g of phosphorus pentasulfide and mix them uniformly and place them in a quartz boat, then put them into a horizontally placed quartz reaction tube (40×1200mm), heat to 700°C under the protection of argon and Leave on for 0.5 hours. After cooling and grinding, a composite catalyst of nickel sulfide and nickel phosphide was obtained, the mass percent content: cobalt 7.2%, nickel 54.5%, sulfur 25.4%, phosphorus 12.9%.

Embodiment 3

[0023] Weigh 0.1g titanium disulfide, evenly spread on 3.5×18cm 2 Put the graphite substrate into a horizontally placed quartz reaction tube (40×1200mm); after vacuuming, fill it with nitrogen and repeat the operation three times; then continuously feed nitrogen with a flow rate of 100mL / min; When the temperature reaches 680°C, hydrogen and ethylene are fed in, and the flow rates are 300mL / min and 120mL / min respectively; after 20 minutes of reaction, the ethylene and hydrogen are stopped, and the heating is stopped; after cooling, take out the graphite substrate, graphite The substrate is covered with fuzzy black matter, namely micro-carbon rolls. Yield 0.46 g. The carbon fiber cross-section of the micro-carbon coil is irregular polygon, the diameter of the carbon fiber is 1.0-1.2 μm, the diameter of the micro-carbon coil is 12-16 μm, the pitch is 2-6 μm, and the length of the micro-carbon coil is 0.5-1.5 mm. The micro-carbon roll has a large stretchability, and is suitable ...

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Abstract

The invention belongs to carbon fiber material, which particular relates to micro carbon roll and its preparation method and use. The invention reaches the realization by looking for the new accelerant to compound micro carbon roll. When use sulphide or phosphide of some transition metal and their composite as accelerant, the reaction, which has no, needs for sulfurous and phosphorus impure substance as accelerant gas, is friendly to environment. The structure of micro carbon roll is similar to DNA, formed by two carbon fiber which curling in same direction; the shape of micro carbon roll is regular and uniform; the radius is 1.5-1.8 mu m; the pitch is 0-6 mu m. It can be used as micro-machined element, micro-electrical element, additive of composite, and wave energy absorbent, which has wide prospect in military and civilian use.

Description

technical field [0001] The invention belongs to the field of carbon fiber materials, and in particular relates to micro-carbon coils and their preparation methods and uses. Background technique [0002] In 1889, US Patent US405480 disclosed the synthesis of carbon fibers. However, due to the lack of advanced technologies such as process control and test characterization at that time, this carbon material has not been well studied. Until the 1980s, with the application of carbon fiber in the fields of polymer additives and catalyst carriers, scientists began to conduct extensive and in-depth research on it. In order to adapt to different uses, a variety of synthesis methods have been developed to obtain carbon fibers with various shapes, properties and performances. Chinese Patent Publication No. CN1078273C discloses the preparation of carbon fiber by flow method, specifically the catalyst ferrocene or Ni(CO) 4 It is fully mixed with the carbon source in the gaseous state, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/12
Inventor 陈丽娟李文军郭燕川徐海涛彭必先
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI