Method for synthesizing carbyne nano-material from calcium carbide and polyhalohydrocarbon as raw materials through ball-milling

A technology of nanomaterials and polyhalogenated hydrocarbons, applied in the application of mechanochemistry in the synthesis of carbon nanomaterials, and the preparation of new alkyne carbon materials, to achieve the effects of excellent physical and chemical properties, uniform texture, and mild reaction conditions

Active Publication Date: 2016-09-21
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0006] In the existing literature and patents, there is no literature report on the preparation of alkyne carbon nanomaterials by ball milling under normal temperature and pressure conditions using calcium carbide and polyhalogenated hydrocarbons as raw materials.

Method used

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  • Method for synthesizing carbyne nano-material from calcium carbide and polyhalohydrocarbon as raw materials through ball-milling
  • Method for synthesizing carbyne nano-material from calcium carbide and polyhalohydrocarbon as raw materials through ball-milling
  • Method for synthesizing carbyne nano-material from calcium carbide and polyhalohydrocarbon as raw materials through ball-milling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 12 grams of 100-mesh calcium carbide (0.141mol) powder and place it in a ball mill jar, and then add 7.2 grams of carbon tetrachloride (0.047mol) to it, and the molar ratio of calcium to halogen is 1.5:2. The ball mill jar was evacuated to a vacuum of 1 kPa, and then placed in a planetary ball mill (QXQM-2, Tianchuang, Changsha). The ball mill was milled for 220 minutes under the condition of the speed of the ball mill at 530 rpm. During the operation, in order to prevent the machine from overheating, stop for 15 minutes every 45 minutes of operation. After the reaction was completed, the ball mill jar was opened, and the original gray powder turned into pitch black, which proved the generation of carbon materials. The reacted product was transferred into a beaker, treated with dilute nitric acid and the chloride ion content in the filtrate was measured, thus confirming that the dechlorination rate of carbon tetrachloride was 95.9%. After acid washing and water wa...

Embodiment 2

[0025] 16 grams of 100-mesh calcium carbide (0.188 mol) powder was placed in a crushing mill (Shanghai Lili), and then 9.85 grams of hexachloroethane (0.041 mol) was added therein three times. Add another 1 / 3 of hexachloroethane after each run for 10 minutes. The accumulative running time is 30min under the rated power. After the reaction was completed, the ball mill jar was opened, and the original gray powder turned into pitch black, which proved the generation of carbon materials. The reacted product was transferred into a beaker, treated with dilute nitric acid and the chloride ion content in the filtrate was measured, thus confirming that the dechlorination rate of hexachloroethane was 99.8%. After the product was acid-washed and washed with water, it was vacuum-dried at 130° C. for 5 hours to obtain the alkyne-carbon material of the present invention. The apparent carbon yield was 110% after weighing and calculating.

[0026] Scanning electron microscope (SEM) test res...

Embodiment 3

[0028] Take 30 grams of 100-mesh calcium carbide (0.352mol) powder and place it in a ball milling jar, then add 9.70 grams of tetrachloroethylene (0.059mol) therein, seal the ball milling jar, and protect it with atmospheric pressure argon. The ball mill jar was placed in a planetary ball mill (QXQM-2, Changsha Tianchuang), and the ball milled at a speed of 530 rpm for 260 minutes. During the operation, the machine was stopped for 15 minutes every 45 minutes to prevent overheating. After the reaction was completed, the ball mill tank was opened to find that the original gray reaction material had turned into a black powder, which proved the generation of carbon materials. Transfer the reacted product into a beaker, treat it with dilute nitric acid and measure the chloride ion content in the filtrate, the dechlorination rate of tetrachlorethylene is 100%. After the product was acid-washed and washed with water, it was vacuum-dried at 130° C. for 5 hours to obtain the alkyne car...

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Abstract

The invention relates to a method for synthesizing a carbyne nano-material from calcium carbide and polyhalohydrocarbon as raw materials through ball-milling and belongs to the field of preparation of novel carbon nano-materials. The method is characterized by comprising the steps: adding the calcium carbide and the polyhalohydrocarbon, which serve as the raw materials for preparing the carbon material, into a ball milling tank in one time or in a staged manner according to a certain ratio, and carrying out a ball-milling reaction for a certain time; and after the reaction ends, subjecting the product to acid washing, and performing water washing and drying, thereby obtaining the carbyne nano-material. According to the method, the reaction raw materials are cheap and readily available, the reaction conditions are mild, and the reaction equipment and process are simple. The produced carbon material is uniform in texture and excellent in physico-chemical properties and has a broad application prospect in the fields of energy, catalysis, environmental protection and the like.

Description

technical field [0001] The invention belongs to the field of preparation of new carbon nanomaterials, in particular to new chemical reactions and high-value utilization of calcium carbide, efficient degradation of polyhalogenated hydrocarbons by calcium carbide, preparation of novel alkyne carbon materials, and mechanochemistry in the synthesis of carbon nanomaterials Applications. Background technique [0002] In the field of science and technology today, the discovery and utilization of new carbon materials is one of the frontiers and research hotspots of materials science. Carbon materials have attracted much attention due to their rich sources of raw materials, diversity of structures and varieties, unique physical and chemical properties, and huge market applications. In recent years, scientists have successively discovered and prepared carbon nanotubes, fullerene C 60 , graphene, graphyne and other new carbon materials, and their unique photoelectric and mechanical p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y40/00
CPCC01P2002/72C01P2002/85C01P2004/03C01P2004/04C01P2004/64
Inventor 李春喜李英杰李文锋刘庆楠
Owner BEIJING UNIV OF CHEM TECH
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