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Process for preparing vapor-grown carbon fibers

A vapor-grown, carbon fiber technology, applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problem that metal particles are not easy to agglomerate, and achieve the effect of uniform, easy to operate, and narrow diameter distribution of vapor-grown carbon fibers.

Inactive Publication Date: 2006-12-06
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In recent years, the research on the application of supported catalysts in the preparation of vapor-phase grown carbon fibers has attracted the general attention of scientific researchers. The advantages of supported catalysts are uniform particles, good dispersion, and metal particles are not easy to aggregate at high temperatures, which can fully play the role of catalysts. , which is conducive to the formation of fibers; but the research mainly focuses on the traditional carrier SiO 2 、Al 2 o 3 (Patent CN03114991, Zhao Tiejun, Gu Xiongyi, Dai Yingchun, Yuan Weikang, transition metal catalyst and method for preparing uniform diameter tubular nano-carbon fiber), and zirconia is less researched as a catalyst carrier for the preparation of vapor-phase grown carbon fiber

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 8.0g of zirconia, add deionized water dropwise to initial moistening, and record the volume of consumed water, 5ml. Based on the final catalyst iron oxide content of 10wt%, weigh 6.7g of iron nitrate, make 5ml of aqueous solution, add all of it to 8.0g of zirconia, soak for 8 hours, dry in the air, and roast at 400°C for 8 hours to obtain the catalyst, which is recorded as cat .1.

[0020] The preparation of gas-phase grown carbon fiber is carried out in a tubular reactor. Weigh 1.0g of catalyst cat.1 and evenly distribute it in a porcelain boat, place it in the reactor, and reduce it in a hydrogen atmosphere. The reduction temperature is 300°C and the time is 6h; When the reaction temperature reached 1100°C, benzene was introduced at a flow rate of 0.020ml / min. After 40 minutes of stabilization, the product in the porcelain boat was collected. The product is a floc, and observed under a scanning electron microscope, the fibers are uniform and the diameter is 2.5...

Embodiment 2

[0022] Weigh 8.0g of zirconia, add deionized water dropwise to initial moistening, and record the volume of consumed water, 5ml. Based on the final catalyst iron oxide content of 20wt%, weigh 16.1g ferric nitrate, make 5ml solution, add all of it into 8.0g zirconia, soak for 40 hours, dry in the air, and roast at 500°C for 4 hours to obtain the catalyst, denoted as cat .2.

[0023] The preparation of gas-phase grown carbon fiber is carried out in a tubular reactor. Weigh 1.0g of catalyst cat.2 and evenly distribute it on the bottom of the porcelain boat, place it in the middle of the reactor, and reduce it in a hydrogen atmosphere. The reduction temperature is 400°C and the time is 4h; Xylene was introduced at 1000°C with a flow rate of 0.040ml / min. After 20 minutes of reaction, the product in the porcelain boat was collected. The observed product is a floc macroscopically, and observed under a scanning electron microscope, the product is a fiber with a diameter of 2.0 μm±5%....

Embodiment 3

[0025] Weigh 11.0 g of zirconia, add deionized water dropwise to initial moistening, and record the consumed water volume of 6 ml. Based on the final catalyst iron oxide content of 35wt%, weigh 32.6g of ferric nitrate, prepare 6ml of solution, add all of it into 11.0g of zirconia, soak for 16 hours, dry in the air, and roast at 600°C for 2 hours to obtain the catalyst, which is recorded as cat. 3.

[0026] The preparation of gas-phase grown carbon fiber is carried out in a tubular reactor. Weigh 1.0g of catalyst cat.3 and evenly distribute it on the bottom of the porcelain boat, place it in the middle of the reactor, and reduce it in a hydrogen atmosphere at a temperature of 500°C for 2 hours; The reaction temperature is 1160°C, and benzene is introduced at a flow rate of 0.030ml / min. After 40 minutes of reaction, the product in the porcelain boat is collected. The product is fluff, and observed under a scanning electron microscope, the product is composed of fibers with a di...

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Abstract

A process for preparing vapor-grown carbon fibers comprises adding 10-35% iron or cobalt oxide and 65-90% zirconia carrier composed of ferric nitrate or cobalt nitrate solution according to weight percent of a catalyzer into the zirconia carrier, and dipping, airing, calcination to obtain the catalyzer. The catalyzer is reduced in a hydric ambience, thereafter the catalyzer's temperature is lifted to a rature 1000-1160 DEG C and a carbon source is entered, an adding amount of the carbon source of a unit quality catalyzer is 0.005-0.040 ml / min, the vapor-grown carbon fibers are obtained by 20-60 minutes reaction. The invention has advantages that the preparing process is simple and easy to operate, the obtained vapor-grown carbon fibers are even, and having a narrow diameter distribution range.

Description

technical field [0001] The invention relates to a preparation method of gas phase growth carbon fiber by using a loaded catalyst. Background technique [0002] Vapor-grown carbon fiber (VGCF) is a kind of high-temperature pyrolysis product of hydrocarbons. It has a series of excellent properties such as high strength, high electrical conductivity, thermal conductivity, low density and unique wave absorption. It is expected to be used as an ultra-high-strength material, lightweight Its growth mechanism, preparation method, properties and applications have attracted people's attention and extensive research. At present, the main preparation method widely used in vapor phase growth carbon fiber is chemical vapor deposition (CVD), that is, under high temperature, hydrocarbons are catalyzed by pyrolysis reaction in the presence of metal catalysts such as iron, cobalt, nickel and their alloys, and deposition is obtained by vapor phase growth. Carbon fibers (Jayasankar M, Chand R,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F9/12
Inventor 刘朗张华史景利郭全贵
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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