CN109553089A - Multi-purpose material heat treatment apparatus - Google Patents

Multi-purpose material heat treatment apparatus Download PDF

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Publication number
CN109553089A
CN109553089A CN201811636010.9A CN201811636010A CN109553089A CN 109553089 A CN109553089 A CN 109553089A CN 201811636010 A CN201811636010 A CN 201811636010A CN 109553089 A CN109553089 A CN 109553089A
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China
Prior art keywords
temperature resistant
heat treatment
treatment apparatus
container
electrode
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CN201811636010.9A
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Chinese (zh)
Inventor
刘媛
薛波
董明
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Sayfo (xuzhou) Co Nano Science And Technology
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Sayfo (xuzhou) Co Nano Science And Technology
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Priority to CN201811636010.9A priority Critical patent/CN109553089A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/168After-treatment
    • C01B32/17Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/168After-treatment
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F17/00Metallocenes
    • C07F17/02Metallocenes of metals of Groups 8, 9 or 10 of the Periodic System
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2202/00Structure or properties of carbon nanotubes
    • C01B2202/20Nanotubes characterized by their properties
    • C01B2202/30Purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A kind of multi-purpose material heat treatment apparatus in materials processing technology field, comprising: inorganic non-metallic high-temperature resistant container, for placing the conductive exothermal element for containing material to be processed;Container is equipped with air inlet and air outlet;The pulse power, power supply positive and negative electrode are connected separately with a high temperature resistant electrode;Two high temperature resistant electrodes connect conduction with conductive exothermal element;Vacuum evacuation device is connected, to container vacuum-pumping with the gas outlet of inorganic non-metallic high-temperature resistant container.The present invention is widely used, can complete fast purifying and the plated film of nano-carbon material in the same apparatus, be conducive to the industrialized production of nano-carbon material and its derived product.

Description

Multi-purpose material heat treatment apparatus
Technical field
The present invention relates to a kind of technology of field of material processing, specifically a kind of multi-purpose material heat treatment is set It is standby.
Background technique
There is unique structure and special physico by the novel nano carbon material of representative of nanotube and nano particle Property is learned, before showing wide application in fields such as Condensed Matter Physics, material science, chemistry and nanoelectronic components Scape.
Industrial production nano-carbon material mainly uses arc process and Floating catalyst method at present, these methods, which facilitate, to be received The acquisition of rice carbon material is provided convenience for the research and practical application of nano-carbon material.However receiving of preparing of the above method Rice carbon material is frequently accompanied by a considerable amount of impurity, and the presence of these impurity greatly hinders the physical property research of nano-carbon material And practical application, therefore more and more attention have been obtained to the purifying research of nano-carbon material.The technical pure of nano-carbon material Change processing method and mainly uses traditional physics, chemical purification methods, such as extraction, thermal decomposition method, oxidation-reduction method, however this The purification efficiency of a little conventional methods is low, and purification quality is not also high;The wherein equipment relative maturity that thermal decomposition method uses, but still There are operating difficulties, the defects of heating time is long, and security risk is big.
Summary of the invention
The present invention In view of the above shortcomings of the prior art, proposes a kind of multi-purpose material heat treatment apparatus, uses Way extensively, fast purifying and the plated film of nano-carbon material can be completed in the same apparatus, be conducive to nano-carbon material and its The industrialized production of derived product, and can be realized the purification of 500 DEG C or less volatizable materials.
The present invention is achieved by the following technical solutions:
The present invention includes:
Inorganic non-metallic high-temperature resistant container, for placing the conductive exothermal element for containing material to be processed;Container be equipped with into Port and gas outlet;
The pulse power, power supply positive and negative electrode are connected separately with a high temperature resistant electrode;Two high temperature resistant electrodes and conductive exothermal element Connection is conductive;
Vacuum evacuation device is connected, to container vacuum-pumping with the gas outlet of inorganic non-metallic high-temperature resistant container.
The conductive exothermal element containing material to be processed is obtained through compacting.
Preferably, the inorganic non-metallic high-temperature resistant container is made of quartz.
The high temperature resistant electrode needs can choose different types of conductive electrode according to processing, for example, graphite electrode, gold Belong to palladium electrode, tungsten-copper alloy electrode.
The inorganic non-metallic high-temperature resistant container is equipped with temperature-measuring port, and the temperature-measuring port is equipped with non-contact temperature measuring device, uses In the temperature of monitoring conductive exothermal element;Preferably, the non-contact temperature measuring device uses optics temperature measurer.
The gas outlet of the inorganic non-metallic high-temperature resistant container is connected with cryotrap, the cooling gas object collected after purification Material.
Technical effect
Compared with prior art, the configuration of the present invention is simple, it is widely used;Based on the good heating conduction of nano-carbon material, Efficient self-heating (the Q=I of nano-carbon material can be realized using pulse current2Rt), the purifying of nano-carbon material is rapidly completed, And can after coating material is added Quick-gasifying coating material, thus nano-carbon material surface carry out plated film processing;And The present invention can also purify the chemical substance of 500 DEG C or less gasifiable (evaporation or distillations) after increasing cryotrap, Such as ferrocene, elemental iodine, sulphur, camphor, borneol, material purity is not less than 99.8% after purification.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of embodiment 1 and embodiment 2;
Fig. 2 is the structural schematic diagram of embodiment 3;
Fig. 3 is the SEM photograph of crystal whisker-shaped multi-walled carbon nanotube in the embodiment of the present invention;
In figure: quartz container 1, conductive exothermal element 2, the pulse power 3, high temperature resistant electrode 4, vacuum evacuation device 5, optics are surveyed Warm instrument 6, cryotrap 7.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention will be described in detail.
Embodiment 1
As shown in Figure 1, the present embodiment is related to a kind of purifier apparatus of carbon nanotube, comprising:
Quartz container 1, for placing the conductive exothermal element 2 for containing material to be processed;Quartz container 1 be equipped with air inlet and Gas outlet;
The pulse power 3, power supply positive and negative electrode are connected separately with a high temperature resistant electrode 4, and high temperature resistant electrode 4 is using Metal Palladium electricity Pole;Two metal palladium electrodes are arranged in quartz container 1;
Vacuum evacuation device 5 is connected with the gas outlet of quartz container 1, vacuumizes to quartz container 1.
The quartz container 1 is equipped with temperature-measuring port, and the temperature-measuring port is equipped with optics temperature measurer 6, for monitoring conductive exothermal member The temperature of part 2.
The present embodiment is used for the purifying of carbon nanotube, specific operation process to be as follows:
S1, conductive exothermal element is made in the compacting of 500g carbon nanotube;Carbon nanotube selects the first element of Suzhou nanometer skill Long 5-10 μm of art Co., Ltd, diameter 50-90nm, purity 90% crystal whisker-shaped multi-walled carbon nanotube, as shown in Figure 3;
S2, conductive exothermal element is placed in quartz container 1, is connect with two metal palladium electrodes;
S3, vacuumize, logical argon gas, repetitive operation 3 times, thoroughly exclude air;It vacuumizes again, makes the vacuum degree of quartz container It is maintained at 9.0 × 10-8mbar;
S4, using pulse Electric heating, it is passed through electric current 1A, current impulse generates joule by metal palladium electrode in 1s Thermal shock, the temperature of carbon nanotube are sharply increased to 500 DEG C, are passed through chlorine at this time, by the iron simple substance and oxygen of carbon nano tube surface Change iron and is oxidized to ferric trichloride, ferric trichloride (315 DEG C of boiling point) gasification discharge;
S5, then lead to nitrogen and foreign gas is discharged, metals content impurity, which is obtained, less than 20ppm, purity is greater than 99.9% High-purity carbon nanotube.
Embodiment 2
The present embodiment and embodiment 1 use identical device, carry out plated film to carbon nanotube;The only material of high temperature resistant electrode It is varied, for the present embodiment using graphite electrode as high temperature resistant electrode, concrete operations are as follows:
S1, crystal whisker-shaped multi-walled carbon nanotube (the first element of Suzhou is weighed respectively in the ratio of carbon silicon mol ratio 1:0.5-2.0 Nanosolutions GmbH, 5-10 μm long, diameter 50-90nm, purity 99%) it is uniformly mixed and is compacted with iodate silicon, it is made and leads Electrical heating element;
S2, conductive exothermal element is placed in quartz container, is connect with two graphite electrodes, then is successively vacuumized, logical argon Gas, repetitive operation 3 times excludes air to thorough, then vacuumizes, and the vacuum degree of quartz container 1 is made to be maintained at 9.0 × 10-8mbar;
S3, it is passed through pulse current, size of current 1A, the current impulse time is 2s, and heating carbon nanotube and iodate silicon are mixed Object is closed to 1100 DEG C, the pyrolysis of iodate silicon forms silicon nanocrystal in carbon nano tube surface, and generates iodine vapor;
S4, there is the carbon nanotube of nano-silicon to be cooled within the scope of 110-200 DEG C coating surface, and logical argon gas purging excludes Plating silicon-carbon nanotube is made in iodine vapor.
Embodiment 3
The present embodiment connects cryotrap 7 on the basis of embodiment 1, in the gas outlet of quartz container 1, while using tungsten Copper alloy electrode replaces metal palladium electrode as high temperature resistant electrode, and for the purification of ferrocene, concrete operations are as follows:
S1, 310g ferrocene (Henan Jie Sen chemical products Co., Ltd, purity 90%) is received with 20g crystal whisker-shaped multi wall carbon Mitron (Suzhou the first element Nanosolutions GmbH, 5-10 μm long, diameter 50-90nm, purity 99%) is uniformly mixed and presses It is real, conductive exothermal element 2 is made;
S2, conductive exothermal element 2 is placed in quartz container 1, is connect with two tungsten-copper alloy electrodes 4;Then vacuumize, Logical argon gas repeats this operation 3 times, thoroughly excludes air, then vacuumize, the vacuum degree of quartz container is made to be maintained at 9.0 × 10- 8mbar;
S3, using pulse electric heating mode, it is passed through electric current 1A, current impulse is generated in 0.2s by tungsten-copper alloy electrode The temperature of joule thermal shock, carbon nanotube and ferrocene mixture is sharply increased to 120 DEG C, ferrocene distillation discharge, in low temperature Condensation-crystallization in cold-trap obtains purity greater than 99.9% high-purity ferrocene, and impurity free iron is deposited in quartz container.
Carbon nanotube can Reusability in the present embodiment.
It is emphasized that: the above is only presently preferred embodiments of the present invention, not make in any form to the present invention Limitation, any simple modification, equivalent change and modification to the above embodiments according to the technical essence of the invention, All of which are still within the scope of the technical scheme of the invention.

Claims (7)

1. a kind of multi-purpose material heat treatment apparatus characterized by comprising
Inorganic non-metallic high-temperature resistant container, for placing the conductive exothermal element for containing material to be processed;Container is equipped with air inlet The gas outlet and;
The pulse power, power supply positive and negative electrode are connected separately with a high temperature resistant electrode;Two high temperature resistant electrodes are connect with conductive exothermal element It is conductive;
Vacuum evacuation device is connected, to container vacuum-pumping with the gas outlet of inorganic non-metallic high-temperature resistant container.
2. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the leading containing material to be processed Electrical heating element is obtained through compacting.
3. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the inorganic non-metallic high temperature resistant is held Device is equipped with temperature-measuring port, and the temperature-measuring port is equipped with non-contact temperature measuring device, for monitoring the temperature of conductive exothermal element.
4. multi-purpose material heat treatment apparatus according to claim 3, characterized in that the non-contact temperature measuring device is adopted With optics temperature measurer.
5. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the inorganic non-metallic high temperature resistant is held The gas outlet of device is connected with cryotrap, the gas material after cooling purification.
6. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the inorganic non-metallic high temperature resistant is held Device is made of quartz.
7. multi-purpose material heat treatment apparatus according to claim 1, characterized in that the high temperature resistant electrode includes graphite One of electrode, metal palladium electrode, tungsten-copper alloy electrode.
CN201811636010.9A 2018-12-29 2018-12-29 Multi-purpose material heat treatment apparatus Pending CN109553089A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110228804A (en) * 2019-07-19 2019-09-13 陕西延长石油(集团)有限责任公司 A kind of carbon nanotube sulphur modification and purification integral method

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CN1436722A (en) * 2003-03-21 2003-08-20 清华大学 Vacuum high-temperature process of purifying carbon nanotube
CN102153069A (en) * 2011-02-25 2011-08-17 中国科学院长春应用化学研究所 Treatment method for nanometer carbon material
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CN111410188A (en) * 2020-06-01 2020-07-14 山东晶石大展纳米科技有限公司 Device and method for directly electrifying and purifying carbon nano tube
CN113443617A (en) * 2021-08-19 2021-09-28 陕西六元碳晶股份有限公司 Continuous carbon nanotube purifying device and process
CN115140729A (en) * 2022-07-18 2022-10-04 株洲弗拉德科技有限公司 Preparation method of high-purity carbon material

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CN1094695A (en) * 1994-05-13 1994-11-09 中国矿业大学北京研究生部 High-temp chlorination refining process for natural graphite
CN1436722A (en) * 2003-03-21 2003-08-20 清华大学 Vacuum high-temperature process of purifying carbon nanotube
CN102190294A (en) * 2010-03-10 2011-09-21 中国科学院大连化学物理研究所 Preparation method for carbon nanotube or graphene nano-carbon material
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CN104192826A (en) * 2014-08-19 2014-12-10 清华大学 Method for improving conductivity of nano carbon material
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CN111410188A (en) * 2020-06-01 2020-07-14 山东晶石大展纳米科技有限公司 Device and method for directly electrifying and purifying carbon nano tube
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Publication number Priority date Publication date Assignee Title
CN110228804A (en) * 2019-07-19 2019-09-13 陕西延长石油(集团)有限责任公司 A kind of carbon nanotube sulphur modification and purification integral method

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