Device and method for preparing graphite by Zn/Fe flame sealed-tube method

A tube sealing method, graphite technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as affecting the efficiency of graphite preparation, time-consuming, etc., to improve practical performance, avoid atmospheric leakage, and improve safety. Effect

Pending Publication Date: 2019-08-20
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The above methods have their own advantages and disadvantages, but the device structure used in the implementation of each method is b

Method used

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  • Device and method for preparing graphite by Zn/Fe flame sealed-tube method
  • Device and method for preparing graphite by Zn/Fe flame sealed-tube method
  • Device and method for preparing graphite by Zn/Fe flame sealed-tube method

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Example Embodiment

[0099] Loading CO 2 Before preparing raw materials, the present invention preferably combines CO 2 The oxidant in the raw material for preparation is decarbonized, and the decarbonization is preferably kept at 800-950°C, more preferably 850-930°C, and even more preferably 900°C; the holding time is preferably 1.5-2.5h, more preferably It is 1.7 to 2.2 hours, more preferably 2 hours.

[0100] CO in the present invention 2 The method of filling, vacuuming, and flame sealing of the raw materials are described in Example 1.

[0101] In the present invention, the CO 2 When heating the raw materials for the preparation, the heating temperature is preferably 840-860°C, more preferably 845-855°C, even more preferably 850°C, and the heating time (ie reaction time) is preferably ≥12h, more preferably 12- 15h, more preferably 13-14h. The heating of the present invention is preferably performed in a muffle furnace.

[0102] When preparing CO 2 When the raw material is an inorganic carbon raw m...

Example Embodiment

[0113] Example 1

[0114] according to Figure 1~2 The structural construction device shown: the main pipeline Z-1 is composed of a 9.5mm outer diameter glass welded high vacuum glass valve (Kimble, USA), and the detachable part is connected with an Ultra-Torr stainless steel joint (Swagelok, USA);

[0115] Vacuum system 1 is supported by Hicube 80 vacuum pump set and compound vacuum gauge PKR 251 (Pfeiffer Vacuum, Germany); the front pump of the turbomolecular pump is an oil-free diaphragm pump;

[0116] First CO 2 Preparation unit 2, second CO 2 Preparation unit 6, the first CO 2 Purification unit 3, second CO 2 Purification unit 5, CO 2 Sampling unit 4 consists of CO 2 Sampling unit 4 consists of CO 2 Constant-volume tube 4-1, double-sleeve reactor 4-2, 13 C sampling pipe 4-3 and backup sample sampling pipe 4-4 are composed, and the setting method is to be fixed at the connecting nozzle of connecting pipe H-2 through a connecting joint;

[0117] The following experiments are carried...

Example Embodiment

[0137] Example 2

[0138] Same as Example 1, except that the inorganic carbon sample is used in the Y-type acidolysis tube with 6mL phosphoric acid (85%V / V, Tianjin Kermel Chemical Reagent) for acidolysis to generate CO 2 . The inorganic carbon sample used in this embodiment is calcite (IHEG Cal, inorganic carbon). The calcite crystals are collected from the Yangliugang Formation (Middle Cambrian ~ 520 Ma), with high crystallinity, pure white and no impurities. The crystals were broken in an agate mortar and soaked in 1% (V / V) hydrochloric acid for 4 hours to remove the influence of surface inorganic carbon. After washing and drying with deionized water, they were used for graphite preparation and carbon dioxide purification and collection.

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Abstract

The invention belongs to the technical field of graphite preparation, and specifically relates to a device and method for preparing graphite by a Zn/Fe flame sealed-tube method. The provided device can shorten the vacuumizing period and improve the CO2 sample collection efficiency. According to the Zn/Fe flame sealed-tube method, Zn powder is taken as a reducing agent, the shortage that when H2 orTiH2 is taken as a reducing agent, methane is generated in the system is overcome; moreover, the flame sealed-tube method can solve the problem that due to long time of an online reducing method, leakage of a vacuum system happens, the background values of the test result are reduced, and the sampling efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of graphite preparation, and in particular relates to a device and a method for preparing graphite by a Zn / Fe flame sealing method. Background technique [0002] With the development and application of accelerator mass spectrometer (AMS), 14 C (half-life 5730ya) isotope dating and tracing technology has provided important technical support for innovative research in many disciplines such as geology, oceanography, environmental science, groundwater science, archaeology and biomedicine, and these applications are all important Established 14 Based on high-precision analysis of C isotopes. [0003] Traditional beta decay counting method measurement 14 At C, it is necessary to convert the sample into benzene for decay counting. This method has the disadvantages of long sample preparation period, large sample volume (>1g carbon), long measurement time, and low test accuracy, which seriously restricts 14 Th...

Claims

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Application Information

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IPC IPC(8): C01B32/205
CPCC01B32/205
Inventor 刘圣华杨庆华史慧霞
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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