CN106512702A - Online purification method for inert gases based on titanium metallic chemical properties - Google Patents
Online purification method for inert gases based on titanium metallic chemical properties Download PDFInfo
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- CN106512702A CN106512702A CN201611136273.4A CN201611136273A CN106512702A CN 106512702 A CN106512702 A CN 106512702A CN 201611136273 A CN201611136273 A CN 201611136273A CN 106512702 A CN106512702 A CN 106512702A
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- titanium
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- purification method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B23/00—Noble gases; Compounds thereof
- C01B23/001—Purification or separation processes of noble gases
- C01B23/0015—Chemical processing only
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0003—Chemical processing
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention belongs to the field of purification for inert gases and especially relates to an online purification method for inert gases based on titanium metallic chemical properties. The online purification method is characterized in that the difference of the chemical properties of metal titanium under high temperature and low temperature states is utilized to purify the inert gases, and meanwhile, the problem of possibility of introducing active materials of the conventional purification method for inert gases can be avoided.
Description
Technical field
The invention belongs to inert gas purge field, more particularly to a kind of noble gases based on titanium chemical property exist
Line purification method.
Background technology
During the spectrum experiment for carrying out laboratory level, it is often desirable to using highly purified noble gases.But by
The maximum vacuum that can be reached in current gas circulation line is about 10-12Pa magnitudes, what is remained in gas circulation line are micro
Oxygen, nitrogen isoreactivity molecule will severely impact the result of spectrum experiment in experimentation, and this is cannot be by selecting high-purity
What noble gases were improved.If the common purification method used in experimental system (for example using Zn-Al pumps, Cu CuO
Deng), will inevitably lead to test the introducing of other active substances such as Zn, Al, Cu in pipeline again, affect the result of experiment.
To overcome above contradiction, the present invention to propose a kind of method of laboratory high-purity noble gases in-line purification, both can be to inertia
Gas carries out in-line purification, can avoid the introducing of the active substance in purification process again, achieved with good in spectrum experiment
Actual effect.
The content of the invention
In order to overcome high-purity noble gases in-line purification in laboratory system to be introduced into active substance in purification process
The contradiction of experiment pipeline, the present invention provide a kind of method of laboratory high-purity noble gases in-line purification.The method can not only
The enough oxygen removed in experiment pipeline, nitrogen isoreactivity molecule, also can avoid the introducing of other active substances in purification process simultaneously.
The content of this method is:Due to titanium, chemical property is highly stable at room temperature, and titanium at high temperature
Chemical property is very active, and which generates covalent bond and ion key compound with halogen and oxygen group elements reaction;With transition elements,
Hydrogen, beryllium, boron family, carbon family and nitrogen group element generate metallic bond compound and limit solid solution;With zirconium, hafnium, vanadium family, chromium race, scandium element
Generate unlimited solid solution;Especially when heating more than 650 DEG C, titanium and oxygen kickback, and when more than 700 DEG C, then with
Also there is kickback in nitrogen.Even but noble gases are not also reacted with titanium at high temperature.
High temperature titanium sponge cleaning system is by rustless steel cylinder, titanium sponge, heater, temperature controller and gas piping composition.Knot
Structure is very simple.
In use, high temperature titanium sponge cleaning system is concatenated in gas circulation line.Noble gases are in gas circulator
In the presence of flow through high temperature titanium sponge cleaning system, remove the impurity such as deoxygenation, nitrogen.
After the purge is complete, if only carrying out experiment using pure inert gas, high temperature titanium sponge cleaning system can be kept
Operation, the purity of noble gases is kept during whole experiment.
Carry out experiment if necessary to the mixture using noble gases with other gases, then can close net with high temperature titanium sponge
Change the pipeline of device connection, open the gas circulation branch road in parallel with high temperature titanium sponge cleaning system, now can be in gas cyclic system
The material needed for the experiment such as halogen is added in system, is used after mixing with noble gases in the presence of gas circulator.Due to
Hardly there is chemical reaction in normal temperature state in titanium, therefore it is non-to be introduced into the micro room temperature titanium of experiment pipeline with any material
It is often stable, do not interfere with the result of experiment.
The present invention has advantages below:
1st, can remove oxygen in gas circulation line after evacuation contained by remaining and experiment noble gases itself,
Nitrogen isoreactivity molecule.
2nd, as room temperature titanium is highly stable, can avoid introducing due to the active substance caused by noble gases in-line purification.
3rd, the method is simple to operate, with low cost.
Description of the drawings
Fig. 1 is the systematic schematic diagram of the embodiment one of the method;
Fig. 2 is the high temperature titanium sponge depurator cross-sectional view used in example one;
Fig. 3 is the spontaneous radiation spectrum of Ne gas before one high-power electron beam pumping of example purification;
Fig. 4 is the spontaneous radiation spectrum of Ne gas after one high-power electron beam pumping of example purification;
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
Example one:Application of this method in electron beam pumping Ne spectrum experiments
(1), as shown in accompanying drawing Fig. 1, each ingredient is as follows for experimental system principle schematic:1- reative cells, 2- quartz windows
Mouthful, 3- scan-type spectrogrphs4- electron accelerators "", 5- photomultiplier detectors6- Tykes
3052B oscillographs, 7- computers, 8- optical fiber, 9- direct reading spectrometer Maya2000Pro, 10- gas circulators, 11- high temperature sea
Continuous titanium inert gas purge device, 12- trigger switch, 13- high voltage power supplies, 14- neons, 15- other gases, 16- vacuum pumps.
(2) using diffusion pump to experimental system evacuation as shown in Figure 1, vacuum reaches 10-7Pa;
(3) it is filled with 99.999% high-purity GB neon 760Torr.Using the neon in the electron-beam excitation air chamber of 150keV
Gas, obtains the spontaneous radiation spectrum of neon using Maya2000Pro direct reading spectrometers, such as Fig. 3 institutes by the quartz window of air chamber
Show;
(4) using diffusion pump to experimental system evacuation as shown in Figure 1, vacuum reaches 10-7Pa;
(5) high temperature titanium sponge depurator is heated to 700 degrees Celsius;
(6) 99.999% high-purity GB neon 760Torr is filled with, high temperature titanium sponge depurator is opened and is entered outlet pipe,
High temperature titanium sponge depurator parallel pipeline is closed, gas circulator is opened 30 minutes.
(7) keep high temperature titanium sponge depurator and gas circulator in running order, swashed using the electron beam of 150keV
The neon got angry in room, obtains the spontaneous spoke of the neon that is excited using Maya2000pro spectrogrphs by the quartz window of air chamber
Spectrum is penetrated, as shown in Figure 4;
(8) by the contrast of Fig. 3 and 4, it can be observed that after using this method, in the experiment of example one, substantially
The radiation spectrum of oxygen and nitrogen can not be observed.About 3 times before the intensity enhancing of the spontaneous radiation spectral line of neon to purification, this is mainly
Due to avoiding quenching effect of the oxygen nitrogen isoreactivity composition to the excited state of neon.
Claims (6)
1. the present invention provides a kind of high-purity noble gases in-line purification method based on titanium chemical property.Its feature exists
In:
Using titanium, under high temperature with low temperature state, the difference of chemical characteristic carries out in-line purification to noble gases.In high tender feeling
Under condition, the chemical property of titanium is very active, chemical reaction can occur with oxygen, nitrogen isoreactivity material, generate solid compounds, so as to
To playing purification by the noble gases on its surface.And at normal temperatures, the chemical property of titanium is highly stable, so as to this
Method can avoid conventional inert method for gas purification may caused by active substance introducing.
2., as described in claim 1, the Titanium used in the purification method can use the metal of titanium sponge or loose structure
The physical aspect of the Titaniums such as titanium, to increase the contact area of the gas and titanium that need to be purified, improves purification efficiency.
3. as described in claim 1, the Titanium used in the purification method can be heated using heater, and can be used
Thermocouple equitemperature detector is measured in real time to the temperature of titanium, and the temperature of Titanium is controlled by temperature controller
System.
4. in the purification method as described in claim 1, the temperature of titanium can be controlled by temperature controller, when need purification
Substance classes it is different when, different heating-up temperatures can be set, to ensure being smoothed out for corresponding chemical reaction.
5. as described in claim 1, based on can be using the gas being in series with gas circulator in the purifier of this purification method
Body pipeline and gas storage system, make the noble gases that need to be purified single or multiple by high-temperature metal titanium, to play good purification
Effect.
6. the Titanium used in the purification method can be placed in the container made by the high temperature stabilizing material such as ceramics, gone forward side by side
Row sealing, is only connected with outer pipeline by entering outlet pipe.
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1050047A (en) * | 1989-09-07 | 1991-03-20 | 安守环 | Non-evaporation type low temp activated degasser and manufacturing process thereof |
US5194233A (en) * | 1990-09-14 | 1993-03-16 | Japan Pionics Co., Ltd. | Process for purification of rare gas |
CN1429658A (en) * | 2001-12-30 | 2003-07-16 | 武汉钢铁集团氧气有限责任公司 | Material for removing impurity in inert gas and its use method |
CN102012333A (en) * | 2009-09-04 | 2011-04-13 | 中国石油化工股份有限公司 | Device for purifying and enriching inert gases and use method |
CN102100999A (en) * | 2009-12-16 | 2011-06-22 | 贵阳铝镁设计研究院 | Method for purifying inert gases and purifying device |
CN104353323A (en) * | 2014-11-12 | 2015-02-18 | 核工业理化工程研究院 | Gas circulating purification device under negative pressure environment |
CN104383784A (en) * | 2014-11-27 | 2015-03-04 | 中国科学技术大学 | System and method for separating and extracting inert gas from environmental gas |
-
2016
- 2016-12-08 CN CN201611136273.4A patent/CN106512702A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1050047A (en) * | 1989-09-07 | 1991-03-20 | 安守环 | Non-evaporation type low temp activated degasser and manufacturing process thereof |
US5194233A (en) * | 1990-09-14 | 1993-03-16 | Japan Pionics Co., Ltd. | Process for purification of rare gas |
CN1429658A (en) * | 2001-12-30 | 2003-07-16 | 武汉钢铁集团氧气有限责任公司 | Material for removing impurity in inert gas and its use method |
CN102012333A (en) * | 2009-09-04 | 2011-04-13 | 中国石油化工股份有限公司 | Device for purifying and enriching inert gases and use method |
CN102100999A (en) * | 2009-12-16 | 2011-06-22 | 贵阳铝镁设计研究院 | Method for purifying inert gases and purifying device |
CN104353323A (en) * | 2014-11-12 | 2015-02-18 | 核工业理化工程研究院 | Gas circulating purification device under negative pressure environment |
CN104383784A (en) * | 2014-11-27 | 2015-03-04 | 中国科学技术大学 | System and method for separating and extracting inert gas from environmental gas |
Non-Patent Citations (1)
Title |
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莫畏等: "《钛合金》", 30 June 1979, 冶金工业出版社 * |
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