CN103449372A - Method for synthetizing chlorine-oxygen compound under low-power microwave plasma condition and adopted synthesizer - Google Patents
Method for synthetizing chlorine-oxygen compound under low-power microwave plasma condition and adopted synthesizer Download PDFInfo
- Publication number
- CN103449372A CN103449372A CN201310369874XA CN201310369874A CN103449372A CN 103449372 A CN103449372 A CN 103449372A CN 201310369874X A CN201310369874X A CN 201310369874XA CN 201310369874 A CN201310369874 A CN 201310369874A CN 103449372 A CN103449372 A CN 103449372A
- Authority
- CN
- China
- Prior art keywords
- chlorine
- oxygen
- plasma
- oxonium compound
- synthesizer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Plasma Technology (AREA)
Abstract
The invention discloses a method for synthetizing a chlorine-oxygen compound under a low-power microwave plasma condition and a synthesizer adopted in the method. The method comprises the following steps: (1) setting a synthetizing system to be in a negative pressure state; (2) introducing argon, adjusting the microwave power, and igniting plasma; (3) introducing oxygen and chlorine into the plasma so as to generate the chlorine-oxygen compound, feeding the chlorine-oxygen compound into an absorption bottle along with a working gas so as to be absorbed by cold water, further absorbing the tail gas by using a buffer bottle with sodium hydroxide; (4) reacting for a while, turning off a microwave power supply, closing a chlorine switch and an argon switch, further feeding oxygen for a little while and subsequently closing an oxygen switch; and (5) sampling and analyzing, measuring the content of the chlorine-oxygen compound, and calculating the yield. According to the method, the plasma (argon) is maintained through low-power microwave, the chlorine and the oxygen are excited because of the microwave plasma, the two gases are interacted to dissociate into atoms or radicals, the atoms or the radicals of the oxygen and the chlorine are regenerated into the chlorine-oxygen compound through composite reaction, and the yield of the chlorine-oxygen compound is or approximate to 90%.
Description
Technical field
The present invention relates to a kind of synthetic method of chlorine oxonium compound, specifically the method for synthetic chlorine oxonium compound and the synthesizer of employing under a kind of low power microwave condition of plasma.
Background technology
The preparation method of tradition chlorine oxonium compound adopts chlorite method and chlorate process.Due to the restriction that is subject to chemical equilibrium and other conversion conditions, create novel process very difficult in the material conversion process under normal condition, simultaneously, greenization has proposed new requirement to technological process.
It is the hertzian wave in the 0.1mm-1m scope that microwave is commonly referred to as wavelength, and its corresponding range of frequency is 300MHz-3000GHz.Plasma body is the molecular ionized gas shape of the positive and negative electricity material that atom after being deprived of by portions of electronics and atom are ionized rear generation, and it is except the solid, liquid, gas state, the 4th state that material exists.Plasma body is a kind of good electrical conductor, utilizes the magnetic field through ingehious design can catch, move and accelerate plasma.
Both at home and abroad the inorganic synthetic research under microwave plasma is also made progress to some extent, as the people such as Yu Aimin use the surface wave excitation Microwave Induced Plasma synthesizer of assembling voluntarily, under normal pressure and mild conditions, the air of take synthesizes oxynitrides as raw material, and the oxynitrides formation mechanism has been carried out to preliminary discussion.The people such as Xu Wenguo have carried out under decompression and room temperature condition, be the research of raw material with microwave plasma synthetic ammonia by hydrogen and nitrogen, and the reaction mechanism of synthetic ammonia has been done to preliminary discussion.
But have not yet to see the method for utilizing under the low power microwave condition of plasma synthetic chlorine oxonium compound and the relevant report of device.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for synthetic chlorine oxonium compound under a kind of low power microwave condition of plasma and the synthesizer of employing, produce the technique of chlorine oxonium compound to break through traditional chlorite method and chlorate process, adopt reaction under non-conventional media low power microwave plasma body to generate chlorine oxonium compound.
The present invention solves the problems of the technologies described above with following technical scheme:
The method of synthetic chlorine oxonium compound under a kind of low power microwave condition of plasma of the present invention, this synthetic method comprises the following steps:
(1) check the synthesizer resistance to air loss, open vacuum system, make system in negative pressure state, after reach-0.1MPa of vacuum tightness, close vacuum system;
(2) after synthesizer is passed into to argon gas, the adjusting microwave power is 120-150W, lights plasma body;
(3) oxygen and chlorine are introduced in plasma body, oxygen and chlorine are excited in argon plasma, through from separating and recombination process generation chlorine oxonium compound, enter in absorption bottle with working gas, then absorb tail gas with the surge flask that sodium hydroxide is housed;
(4) after reaction 30-60min, close microwave power supply, chlorine, argon gas switch, after logical 1-2min oxygen, close again oxygen switch;
(5) sampling analysis, the content of mensuration chlorine oxonium compound, calculate the chlorine oxonium compound productive rate.
In above-mentioned steps (2), the argon flow amount passed into is 0.8-1mL/s.
In above-mentioned steps (3), the flow of oxygen and chlorine is respectively 0.6-0.75mL/s and 0.25-0.4mL/s.
7-10 ℃ of cold water is housed in above-mentioned absorption bottle.
The synthesizer that under low power microwave condition of plasma of the present invention, the method for synthetic chlorine oxonium compound adopts, mainly by surface wave excitation device, absorption bottle, surge flask and vacuum system, formed, the surface wave excitation device connects microwave power supply, the surface wave excitation device is built-in with quartz discharge tube, quartz discharge tube connects the input channel of argon gas, oxygen and chlorine generating unit, the output terminal of quartz discharge tube connects absorption bottle by the road, absorption bottle is connected with the surge flask that sodium hydroxide is housed by the road, and surge flask connects vacuum system.
Described absorption bottle is provided with two, and forms and be connected in series by pipeline.
The present invention has following advantage :) the present invention is under the condition of non-conventional media plasma body, utilize low power microwave to maintain plasma body (argon gas), chlorine and oxygen are excited, in the argon microwave plasma, each main active component has higher energy, and be far longer than each chemical bond dissociation energy of oxygen and chlorine molecule, active ingredient in argon plasma can interact and make it be dissociated into atom (Cl or O) or (free radical Cl with oxygen and chlorine, O), atom or the free radical of these oxygen and chlorine generate chlorine oxonium compound by complex reaction again, the productive rate of chlorine oxonium compound reaches or approaches 90%.2) synthetic method of the present invention is compared with the chlorite method with traditional chlorate process, does not have a large amount of by products to produce, and is a kind of method of environmental protection Sustainable development.
The accompanying drawing explanation
Fig. 1 is the schematic flow sheet of synthetic chlorine oxonium compound under low power microwave condition of plasma of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
The synthesizer that under low power microwave condition of plasma of the present invention, the method for synthetic chlorine oxonium compound adopts, mainly by surface wave excitation device 3, absorption bottle 6, absorption bottle 7, surge flask 8 and vacuum system 9 form, surface wave excitation device 3 connects microwave power supply, surface wave excitation device 3 is built-in with quartz discharge tube 4, quartz discharge tube 4 connects argon gas, the input channel of oxygen and chlorine generating unit, the output terminal of quartz discharge tube 3 connects absorption bottle 6 by the road, absorption bottle 6 connects absorption bottle 7 by the road, absorption bottle 7 connects the surge flask 8 that sodium hydroxide is housed by the road, surge flask 8 connects vacuum system 9.
The concrete operations of synthesizer of the present invention are as follows:
Check the resistance to air loss of synthesizer, open vacuum system 9, the vacuum tightness of system is reached-0.1MPa, close vacuum system.Open the needle-valve 1 of controlling argon gas, the flow velocity that argon gas is controlled in adjust flux agent 2 is 0.8-1mL/s, opens microwave power supply, lights plasma body 5.Open the needle-valve of controlling oxygen and chlorine, the adjust flux agent, the flow velocity with 0.6-0.75mL/s and 0.25-0.4mL/s is logical by oxygen and chlorine introducing plasma body respectively.Owing to reaching 120W-150W when microwave power, plasma body is broken through the restriction of surface wave excitation device 3 cavitys, along quartz discharge tube 4 internal surfaces, stretch out, in system, oxygen and chlorine are excited in argon plasma, through from solution and recombination process, generating chlorine oxonium compound, and enter in absorption bottle 6 and 7 and be absorbed with working gas, 7-10 ℃ of cold water is housed in absorption bottle.Owing to producing chlorine oxonium compound and unreacted chlorine meeting polluted air in experiment, so need to absorb tail gas with the surge flask 8 that sodium hydroxide is housed, close microwave power supply, chlorine, argon gas switch after reaction 30-60min, owing to also having retained chlorine oxonium compound and chlorine in system, so just close oxygen switch after need to leading to again 1-2min oxygen.Sampling analysis, the content of mensuration chlorine oxonium compound, calculate productive rate.
The outstanding feature that is produced microwave plasma by microwave excitation surface wave excitation device is the restriction that microwave plasma can be broken through the cavity own vol, and along with the increase of microwave power, plasma body can stretch out along discharge tube.The effect of microwave-excitation circuit is to cause ionization, forms initial plasma body, and has encouraged surface-duided wave again on the interface of medium tube and plasma body, and this surface-duided wave can make plasma body continuation and stable simultaneously.
Plasma body maintains in quartz discharge tube, along with the input microwave power increases, plasma body also corresponding increase of density.Active ingredient in argon plasma can interact and make it be dissociated into atom or free radical with oxygen and chlorine, and atom or the free radical of these oxygen and chlorine generate chlorine oxonium compound by complex reaction again, after be collected the device absorption.
Below embodiments of the invention:
Check the synthesizer resistance to air loss, open vacuum system, after reach-0.1MPa of the vacuum tightness of system, close vacuum system, with 0.9mL/s, pass into argon gas, the adjusting microwave power is 140W, lights plasma body.Flow velocity with 0.65mL/s and 0.3mL/s passes in oxygen and chlorine introducing plasma body respectively, oxygen and chlorine are excited in argon plasma, through from solution and recombination process, generating chlorine oxonium compound, and enter in absorption bottle with working gas, 7 ℃ of cold water are housed in absorption bottle, and absorb tail gas with the surge flask that sodium hydroxide is housed, and close microwave power supply, chlorine, argon gas switch after reaction 40min, close again oxygen switch after logical 1min oxygen.Sampling analysis, the content of mensuration chlorine oxonium compound, the productive rate of chlorine oxonium compound reaches 88%.
The inspection units resistance to air loss, open vacuum system, after reach-0.1MPa of the vacuum tightness of system, closes vacuum system, with 1mL/s, passes into argon gas, and the adjusting microwave power is 130W, lights plasma body.Flow velocity with 0.7mL/s and 0.4mL/s passes in oxygen and chlorine introducing plasma body respectively, oxygen and chlorine are excited in argon plasma, through from solution and recombination process, generating chlorine oxonium compound, and enter in absorption bottle with working gas, 8 ℃ of cold water are housed in absorption bottle, and absorb tail gas with the surge flask that sodium hydroxide is housed, and close microwave power supply, chlorine, argon gas switch after reaction 50min, close again oxygen switch after logical 1.5min oxygen.Sampling analysis, the content of mensuration chlorine oxonium compound, the productive rate of chlorine oxonium compound reaches 89%.
Embodiment 3
The inspection units resistance to air loss, open vacuum system, after reach-0.1MPa of the vacuum tightness of system, closes vacuum system, with 0.8mL/s, passes into argon gas, and the adjusting microwave power is 150W, lights plasma body.Flow velocity with 0.75mL/s and 0.35mL/s passes in oxygen and chlorine introducing plasma body respectively, oxygen and chlorine are excited in argon plasma, through from solution and recombination process, generating chlorine oxonium compound, and enter in absorption bottle with working gas, 10 ℃ of cold water are housed in absorption bottle, and absorb tail gas with the surge flask that sodium hydroxide is housed, and close microwave power supply, chlorine, argon gas switch after reaction 60min, close again oxygen switch after logical 2min oxygen.Sampling analysis, the content of mensuration chlorine oxonium compound, the productive rate of chlorine oxonium compound reaches 90%.
Claims (6)
1. the method for synthetic chlorine oxonium compound under a low power microwave condition of plasma, is characterized in that, this synthetic method comprises the following steps:
(1) check the synthesizer resistance to air loss, open vacuum system, make system in negative pressure state, after reach-0.1MPa of vacuum tightness, close vacuum system;
(2) after synthesizer is passed into to argon gas, the adjusting microwave power is 120-150W, lights plasma body;
(3) oxygen and chlorine are introduced in plasma body, oxygen and chlorine are excited in argon plasma, through from separating and recombination process generation chlorine oxonium compound, enter in absorption bottle with working gas, then absorb tail gas with the surge flask that sodium hydroxide is housed;
(4) after reaction 30-60min, close microwave power supply, chlorine, argon gas switch, after logical 1-2min oxygen, close again oxygen switch;
(5) sampling analysis, the content of mensuration chlorine oxonium compound, calculate the chlorine oxonium compound productive rate.
2. the method for synthetic chlorine oxonium compound under the low power microwave condition of plasma according to claim 1, is characterized in that, in step (2), the argon flow amount passed into is 0.8-1mL/s.
3. the method for synthetic chlorine oxonium compound under the low power microwave condition of plasma according to claim 1, is characterized in that, in step (3), the flow of oxygen and chlorine is respectively 0.6-0.75mL/s and 0.25-0.4mL/s.
4. the method for synthetic chlorine oxonium compound under the low power microwave condition of plasma according to claim 1, is characterized in that, 7-10 ℃ of cold water is housed in described absorption bottle.
5. the synthesizer that under a low power microwave condition of plasma, the method for synthetic chlorine oxonium compound adopts, it is characterized in that, described synthesizer mainly is comprised of surface wave excitation device, absorption bottle, surge flask and vacuum system, the surface wave excitation device connects microwave power supply, the surface wave excitation device is built-in with quartz discharge tube, quartz discharge tube connects the input channel of argon gas, oxygen and chlorine generating unit, the output terminal of quartz discharge tube connects absorption bottle, absorption bottle is connected with the surge flask that sodium hydroxide is housed by the road, and surge flask connects vacuum system.
6. the synthesizer that the method for synthetic chlorine oxonium compound adopts under the low power microwave condition of plasma according to claim 5 is characterized in that described absorption bottle is provided with two, and forms and be connected in series by pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310369874XA CN103449372A (en) | 2013-08-22 | 2013-08-22 | Method for synthetizing chlorine-oxygen compound under low-power microwave plasma condition and adopted synthesizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310369874XA CN103449372A (en) | 2013-08-22 | 2013-08-22 | Method for synthetizing chlorine-oxygen compound under low-power microwave plasma condition and adopted synthesizer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103449372A true CN103449372A (en) | 2013-12-18 |
Family
ID=49732279
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310369874XA Pending CN103449372A (en) | 2013-08-22 | 2013-08-22 | Method for synthetizing chlorine-oxygen compound under low-power microwave plasma condition and adopted synthesizer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103449372A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621362A (en) * | 2014-11-05 | 2016-06-01 | 中国科学院大连化学物理研究所 | Oxyiodide preparation apparatus capable of increasing single heavy-state oxygen yield and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4472254A (en) * | 1983-05-02 | 1984-09-18 | Olin Corporation | Electric plasma discharge combustion synthesis of chlorine dioxide |
| CN2498139Y (en) * | 2001-08-09 | 2002-07-03 | 林映津 | Automatic chlorine dioxide generator with microwave heating |
| CN2714535Y (en) * | 2004-07-13 | 2005-08-03 | 荆树明 | Chlorine dioxide generator |
| CN102275878A (en) * | 2010-06-11 | 2011-12-14 | 广西博世科环保科技股份有限公司 | Low-acidity energy-saving production process for high-purity chlorine dioxide |
| CN102381711A (en) * | 2011-07-05 | 2012-03-21 | 兰州大学 | Method for purifying metallurgical-grade polycrystalline silicon by using microwave plasmas |
-
2013
- 2013-08-22 CN CN201310369874XA patent/CN103449372A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4472254A (en) * | 1983-05-02 | 1984-09-18 | Olin Corporation | Electric plasma discharge combustion synthesis of chlorine dioxide |
| CN2498139Y (en) * | 2001-08-09 | 2002-07-03 | 林映津 | Automatic chlorine dioxide generator with microwave heating |
| CN2714535Y (en) * | 2004-07-13 | 2005-08-03 | 荆树明 | Chlorine dioxide generator |
| CN102275878A (en) * | 2010-06-11 | 2011-12-14 | 广西博世科环保科技股份有限公司 | Low-acidity energy-saving production process for high-purity chlorine dioxide |
| CN102381711A (en) * | 2011-07-05 | 2012-03-21 | 兰州大学 | Method for purifying metallurgical-grade polycrystalline silicon by using microwave plasmas |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621362A (en) * | 2014-11-05 | 2016-06-01 | 中国科学院大连化学物理研究所 | Oxyiodide preparation apparatus capable of increasing single heavy-state oxygen yield and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101648698B (en) | Preparation method of high purity hydrogen | |
| CN103204466A (en) | Device and method for preparing hydrogen through temperature controlled continuous decomposition of hydrogen sulfide | |
| PL374947A1 (en) | Pulse gasification and hot gas cleanup apparatus and process | |
| RU2006134642A (en) | METHOD AND DEVICE FOR CONVERSION OF HYDROGEN SULFUR TO HYDROGEN AND SULFUR | |
| CN204733447U (en) | A kind of plasma torch | |
| CN103449372A (en) | Method for synthetizing chlorine-oxygen compound under low-power microwave plasma condition and adopted synthesizer | |
| CN102371888A (en) | Vehicle-mounted plasma generator for purifying nitric oxide in vehicle tail gas | |
| WO2004092548A3 (en) | Portable heat and gaseous fuel generator that does not require electrical power input or electrical control | |
| CN103130182A (en) | Method for increasing hydrogen desorption capacity by sodium borohydride through hydrolysis | |
| CN103537168A (en) | Process for reducing pressure in pressure swing adsorption tower during desorption | |
| CN203862112U (en) | Hydrogen fluoride gas purification device for rare earth | |
| CN113072426B (en) | Method and device for synthesizing methanol by using carbon dioxide and methane | |
| CN103318840B (en) | Magnesium-based composite hydrogen-storage material, and preparation method and application thereof | |
| CN202989293U (en) | Efficient exchange membrane water electrolysis hydrogen production device | |
| CN202968507U (en) | Device for removing oxygen from marsh gas based on plasma reactor | |
| CN201750986U (en) | Harmless treatment system using microwave plasmas for decomposing Freon | |
| CN112211801B (en) | Efficient air compression device and method based on gas adsorption and desorption effects | |
| CN103007678A (en) | Ozone disinfection oxygenerator | |
| CN208943805U (en) | Sulfur hexafluoride degradation treatment device based on dielectric barrier discharge | |
| CN102869182A (en) | Large-volume microwave plasma generating device based on coupling window radiation | |
| CN104261413B (en) | Plasma deoxidization in low termprature producing trichlorosilane by using silicon tetrachloride method and device thereof | |
| CN203976393U (en) | A kind of novel ultra-pure hydrogen producer | |
| CN103007674A (en) | Composite high concentration oxygenerator based on combining molecular size arrangement priority filtering technology with pressure swing adsorption oxygen generating technology | |
| CN205023850U (en) | High -efficiency ozone generator | |
| CN102794146B (en) | Microwave plasma reaction device for preparing nano-material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131218 |