CN100393612C - Method of fixing nitrogen in water and its device - Google Patents
Method of fixing nitrogen in water and its device Download PDFInfo
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- CN100393612C CN100393612C CNB2006100863957A CN200610086395A CN100393612C CN 100393612 C CN100393612 C CN 100393612C CN B2006100863957 A CNB2006100863957 A CN B2006100863957A CN 200610086395 A CN200610086395 A CN 200610086395A CN 100393612 C CN100393612 C CN 100393612C
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Abstract
The present invention discloses a method for making nitrogen fixation in water and its device. It is characterized by that the nitrogen-contained gas is aerated into water, at the same time the high-voltage pulse discharge is made, the discharge electrode is positioned in the water. The pulse width of the described pulse discharge is 200-500 NS, the rise advancing edge of pulse voltage is less than 20 NS, the pulse frequency is greater than 50H2, peak voltage is greater than 10 KV and discharge time is above 3 min so as to obtain nitric acid solution. The device using said method includes the following several portions: gas chamber positioned in the bottom portion of main reaction chamber, several aeration micropores and several upwards-projected needle discharge electrodes which are set in the top portion of gas chamber, grounding electrode placed in said main reaction chamber, the output of high-voltage pulse power supply is respectively connected with discharge electrode and grounding electrode.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogen compound, be specifically related to a kind of preparation method and device thereof that directly nitrogen is changed into nitric acid in water.
Background technology
Airborne nitrogen is fixed up and is converted into the form that can be utilized, become in 20 beginnings of the century that many scientists pay close attention to and key subjects deeply concerned.At present, the method for technical azotification is mainly Haber-Bu and excutes a law (haber-bosch), utilizes catalyzer, under suitable temperature and pressure, with hydrogen and nitrogen with three to one ratio synthetic ammonia.The required temperature of this method is between 450 to 600 degree Celsius, and improved method can be carried out between 350 to 400 degree Celsius, and required pressure is usually between 300 to 600 normal atmosphere, thereby complex manufacturing, energy consumption are big.Thereby, people are seeking other fixed nitrogen method always, as, Wang Yan etc. are at " Dalian Maritime University's journal " 2002.5, disclose " strong ionization discharge synthetic ammonia experimental study " literary composition, utilized strong ionization discharge under gaseous state, will to synthesize ammonia after nitrogen and the hydrogen gas ionizes at normal temperatures and pressures.This method can be carried out at normal temperatures and pressures, but the concentration of acquisition synthetic ammonia is still undesirable.
Simultaneously, adopt aforesaid method synthetic ammonia, the product ammonia of acquisition is converted into nitric acid as primary products mostly and just is used as the nitrogenous source in the Industrial processes afterwards in chemical fertilizer industry, man-made fiber and plastics industry and explosive manufacturing processed.
Therefore, if in the process of fixed nitrogen, nitric acid will bring strategic innovation for inorganic chemical industry industry as the direct first product of technical azotification.Yet, how to impel nitrogen fixed nitrogen to be nitric acid in the certain technology of liquid phase utilization, be the problem that needs solution at present.
Plasma body mainly by the ionization of gas generation, can excite, the activated gas molecule, makes it have reactive behavior, and therefore, discharge low-temperature plasma is applied to the conversion of the metastable gas molecule of chemical property or becomes an important field of research.In the prior art, the report that utilizes strong ionization discharge to synthesize gases such as acetylene, ammonia, ethene is arranged under gaseous state.
Discharge plasma has caused concern widely in the outstanding progress of numerous areas, and some scholars are applied to liquid phase to this technology and form discharge in water, are mainly used to the organic pollutant of bio-refractory in the degradation water.Some laboratories prove that in succession the high-voltage pulse discharge in water can successfully be realized the removal of organic pollutant in the water, and this technology of Clements first Application has been carried out the decolorization experiment of waste water.But in these work, Shang Weijian utilizes the report of discharge plasma technique nitric acid synthesis in water.
Summary of the invention
The object of the invention provides the method that a kind of technology is simple, the nitrogen in the source of the gas directly can be fixed as nitric acid in water, to make things convenient for the utilization of nitrogen.
For achieving the above object, the technical solution used in the present invention is: the method for fixed nitrogen in a kind of water, Xiang Shuizhong exposes to the sun with nitrogenous gas, carries out high pressure pulse discharge simultaneously, and discharge electrode is in water, the pulsewidth of described impulsive discharge is between 200～500 nanoseconds, the rising front of pulsed voltage is less than 200 nanoseconds, and pulse-repetition is greater than 50Hz, and crest voltage is greater than 10 kilovolts, be no less than 3 minutes discharge time, obtain salpeter solution.
In the technique scheme,, impel nitrogen ionization in discharge process to form nitrogen plasma, bring out the liquid phase plasma chemical reaction, generate nitric acid, realized nitrogen directly fixing in water by high pressure pulse discharge.Wherein, also contain materials such as nitrous acid in the solution of acquisition, can further transform or purification by prior art.
In the technique scheme, discharge electrode is in water, and ground-electrode then can arrange as required, nitrogenous gas is exposed to the sun between above-mentioned two electrodes get final product in the entry.Can be, the ground-electrode of described high pressure pulse discharge be in water, and forms discharge in water; Also can be that the ground-electrode of described high pressure pulse discharge is positioned at water surface top, forms gas-liquid mixed discharge.
Wherein, described nitrogenous gas is a nitrogen; Or air.
The device of fixed nitrogen in a kind of water of realization aforesaid method, comprise reaction vessel, cooling system and power supply, chamber in the described reaction vessel comprises main reaction chamber, be positioned at the main reaction chamber bottom air chamber, be positioned at the water coolant compartment of main reaction chamber periphery, described air chamber is communicated with source of the gas, the air chamber top is provided with a plurality of aerating pores and a plurality of pin shaped electric discharging electrodes to upper process, described water coolant compartment is communicated with cooling system, be provided with ground-electrode in the described main reaction chamber, described power supply is a high-voltage pulse power source, and its output is electrically connected with discharge electrode and ground-electrode respectively.
In the technique scheme, described power supply is used to export high-voltage pulse, can adopt prior art to make, for example, after (0-50 kilovolt) boosted through transformer by industrial-frequency alternating current, the ac high-voltage of acquisition obtained the less high direct voltage of pulsing through full-wave rectification and capacitor filtering, this high direct voltage is charged to pulse electric capacity through current-limiting inductance and unidirectional silicon stack, by rotary gap or thyratron high voltage pulse is imported main reaction chamber at last.This power supply architecture is a prior art, comprises single spark gap structure, two spark gap structure or thyratron one pulse transformer structure, all goes for the technical program.Wherein, discharge realizes that by discharge electrode and ground-electrode discharge electrode is made of a plurality of needle electrodes usually, and ground-electrode both can be a pole plate, also can be polar net.In main reaction chamber, the height of ground electrode arrangement can be according to actual set, for example, can set lowlyer, immerse in the water when making reaction, thereby realize pulsed-liquid phase discharge, also can set higherly, during reaction above the water surface, thereby realize gas-liquid mixed discharge.
In the technique scheme, described main reaction chamber top is provided with lid, is provided with the grounding screw rod that penetrates lid, and the ground-electrode in grounding screw rod lower end and the main reaction chamber is connected, and the upper end is connected with the cathodic electricity of high-voltage pulse power source, has the gas evolution mouth on the lid.
The bottom that aerating pore stretches into main reaction chamber is passed at the tip of described pin shaped electric discharging electrodes.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. the present invention is by exposing to the sun in the discharge in water reactor to contain the gas of source nitrogen, impel nitrogen ionization in discharge process to form nitrogen plasma, bring out the liquid phase plasma chemical reaction, generate nitric acid, realized nitrogen directly fixing in water, solved in the prior art at first synthetic ammonia, be converted into the problem that just is used as the nitrogenous source in the Industrial processes after the nitric acid again, technological process is simple;
2. because the present invention obtains nitric acid by a step, nitrogenous source utilizes cost low;
3. device of the present invention exposes to the sun into nitrogen by the solarization air cap of bottom, and acicular discharge electrode is stretched out from sudden and violent solarization air cap, makes nitrogen can pass through liquid phase (or gas-liquid) region of discharge more effectively, has guaranteed normally carrying out of reaction.
Description of drawings
Accompanying drawing 2 is the principle schematic of a kind of single spark gap power supply of use among the embodiment one;
Accompanying drawing 3 is liquid phase NO when exposing to the sun air among the embodiment one
2 -, NO
3 -The change in concentration synoptic diagram;
Accompanying drawing 4 is liquid phase NO when exposing to the sun nitrogen among the embodiment one
2 -, NO
3 -The change in concentration synoptic diagram;
Accompanying drawing 5 is the apparatus structure synoptic diagram of the embodiment of the invention two;
Accompanying drawing 6 is the apparatus structure synoptic diagram of the embodiment of the invention three.
Wherein: 1, main reaction chamber; 2, air chamber; 3, water coolant compartment; 4, gas blower; 5, under meter; 6, aerating pore; 7, discharge electrode; 8, cooling-water pump; 9, heat exchange container; 10, ground connection pole plate; 11, grounding screw rod; 12, lid; 13, gas evolution mouth; 14, ground connection polar net.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment one: referring to accompanying drawing 1 to shown in the accompanying drawing 4, the device of fixed nitrogen in a kind of water, comprise reaction vessel, cooling system and power supply, chamber in the described reaction vessel comprises main reaction chamber 1, be positioned at the air chamber 2 of main reaction chamber bottom, be positioned at the water coolant compartment 3 of main reaction chamber periphery, described air chamber is communicated with source of the gas, in the present embodiment, source of the gas can be gas blower 4, under meter 5 is set on intake ducting, the air chamber top is provided with a plurality of aerating pores 6 and a plurality of pin shaped electric discharging electrodes 7 to upper process, the bottom that aerating pore 6 stretches into main reaction chamber 1 is passed at the tip of pin shaped electric discharging electrodes 7, described water coolant compartment is communicated with cooling system, be provided with ground-electrode in the described main reaction chamber 1, described power supply is a high-voltage pulse power source, and its output is electrically connected with discharge electrode 7 and ground-electrode respectively.
In the present embodiment, the tabular metal ground connection pole plate 10 that described ground-electrode is arranged horizontally, main reaction chamber 1 top is provided with lid 12, be provided with the grounding screw rod 11 that penetrates lid, ground connection pole plate in grounding screw rod 11 lower ends and the main reaction chamber is connected, the upper end is connected with the cathodic electricity of high-voltage pulse power source, has gas evolution mouth 13 on the lid.Cooling system can adopt the general cooling system that is made of cooling-water pump 8, heat exchange container 9 and corresponding pipeline.
Adopt the device of present embodiment to carry out fixed nitrogen in the water, in main reaction chamber, add water, discharge electrode is in water, opens cooling system, Xiang Shuizhong exposes to the sun with air, carry out high pressure pulse discharge simultaneously, form discharge in water, the pulsewidth of described impulsive discharge is between 200～500 nanoseconds, and the rising front of pulsed voltage is less than 200 nanoseconds, crest voltage is greater than 10 kilovolts, the NO that the exoelectrical reaction different time records
2 -, NO
3 -The change in concentration situation as shown in Figure 3.
Change Xiang Shuizhong into and expose to the sun with nitrogen, the change in concentration situation as shown in Figure 4.
In the device of present embodiment, the main component parameter of power-supply system is: and transformer (0-50kV, 1250VA), filter capacitor, 1 μ F; Pulsed capacitance, 2000pF;
The power supply output parameter is: crest voltage, 12KV; Pulse-repetition, 150Hz; Pulsewidth, 200～500ns; Rising front, 60ns.
Input reactor power is 54.2W; Aeration flow: 60L/h; Reactor water sample volume, 100mL.
From accompanying drawing 3 and accompanying drawing 4 as seen, initial reaction stage, the N0 that generates in the liquid phase
2 -More relatively, but after reaction 7 to 9 minutes, NO
3 -Concentration begin to surpass NO
2 -, final product is based on nitric acid.Discharge 21 minutes the time, liquid phase fixed nitrogen product accounts for 95% based on nitric acid.The concentration of nitric acid is respectively: the air that exposes to the sun, 1.36 * 10
-3Mol/L; The pure nitrogen gas that exposes to the sun, 1.53 * 10
-3Mol/L.The productive rate of nitric acid (output that refers to nitric acid under the unit intake) is: when exposing to the sun air, and 1.99 * 10
-9Mol/J; When exposing to the sun nitrogen, 2.24 * 10
-9Mol/J.
Embodiment two: shown in accompanying drawing 5, the device of fixed nitrogen in a kind of water, comprise reaction vessel, cooling system and power supply, chamber in the described reaction vessel comprises main reaction chamber 1, be positioned at the air chamber 2 of main reaction chamber bottom, be arranged in the water coolant compartment (figure does not draw) of main reaction chamber periphery, described air chamber is communicated with source of the gas, in the present embodiment, source of the gas can be gas blower 4, the air chamber top is provided with a plurality of aerating pores 6 and a plurality of pin shaped electric discharging electrodes 7 to upper process, the bottom that aerating pore stretches into main reaction chamber is passed at the tip of pin shaped electric discharging electrodes, described water coolant compartment is communicated with cooling system, be provided with ground-electrode in the described main reaction chamber, described power supply is a high-voltage pulse power source, and its output is electrically connected with discharge electrode and ground-electrode respectively.
In the present embodiment, the netted metal ground connection polar net 14 that described ground-electrode is arranged horizontally, ground connection polar net periphery can be fixed with the main reaction chamber container, the main reaction chamber top is provided with lid 12, be provided with the grounding screw rod 11 that penetrates lid, ground connection polar net 14 in grounding screw rod lower end and the main reaction chamber is connected, and the upper end is connected with the cathodic electricity of high-voltage pulse power source, has gas evolution mouth 13 on the lid.
The main component parameter of power-supply system is: and high pressure producer (0-40kV, 120VA), filter capacitor, 2000pF; Pulsed capacitance, 1200pF;
Implementation process power supply output parameter is: crest voltage, 28KV; Pulse-repetition, 150Hz; Pulsewidth, 500ns; Rising front, 60ns.
Input reactor power is 35.3W; Aeration flow: 120L/h; Reactor water sample volume, 300mL.
Discharge 36 minutes the time, liquid phase fixed nitrogen product accounts for 99% based on nitric acid.When exposing to the sun air, discharged 36 minutes, the concentration of nitric acid is 1.96 * 10
-3Mol/L, the productive rate of nitric acid is: 2.57 * 10
-8Mol/J.
Embodiment three: shown in accompanying drawing 6, the device of fixed nitrogen in a kind of water, comprise reaction vessel, cooling system and power supply, chamber in the described reaction vessel comprises main reaction chamber 1, be positioned at the air chamber 2 of main reaction chamber bottom, be arranged in the water coolant compartment (figure does not draw) of main reaction chamber periphery, described air chamber is communicated with source of the gas, in the present embodiment, source of the gas can be gas blower 4, the air chamber top is provided with a plurality of aerating pores 6 and a plurality of pin shaped electric discharging electrodes 7 to upper process, the bottom that aerating pore stretches into main reaction chamber 1 is passed at the tip of pin shaped electric discharging electrodes, described water coolant compartment is communicated with cooling system, be provided with ground-electrode in the described main reaction chamber, described power supply is a high-voltage pulse power source, and its output is electrically connected with discharge electrode and ground-electrode respectively.
In the present embodiment, the metal ground connection pole plate 10 that described ground-electrode is arranged horizontally, the main reaction chamber top is provided with lid 12, be provided with the grounding screw rod 11 that penetrates lid, ground connection pole plate in grounding screw rod lower end and the main reaction chamber 1 is connected and fixed, the upper end is connected with the cathodic electricity of high-voltage pulse power source, has gas evolution mouth 13 on the lid.Discharge electrode 7 is arranged in the top of main reaction chamber water, forms gas-liquid mixed discharge thus.
The main component parameter of power-supply system is: and high pressure producer (0-40kV, 120VA), filter capacitor, 2000pF; Pulsed capacitance, 1200pF;
Implementation process power supply output parameter is: crest voltage, 28KV; Pulse-repetition, 150Hz; Pulsewidth, 500ns; Rising front, 60ns.
Input reactor power is 35.3W; The aeration flow; 120L/h; Reactor water sample volume, 300mL.
Discharge 36 minutes the time, liquid phase fixed nitrogen product is based on nitric acid.When exposing to the sun air, discharge 36 minutes the time, the concentration of nitric acid is 1.76 * 10
-3About mol/L, the productive rate of nitric acid is: 2.31 * 10
-8About mol/J.
Claims (8)
1. the method for fixed nitrogen in the water, it is characterized in that: Xiang Shuizhong exposes to the sun with nitrogenous gas, carry out high pressure pulse discharge simultaneously, discharge electrode is in water, and the pulsewidth of described pulsed voltage is between 200～500 nanoseconds, and the rising front of pulsed voltage is less than 200 nanoseconds, pulse-repetition is greater than 50Hz, crest voltage is no less than 3 minutes discharge time greater than 10 kilovolts, obtains dilute nitric acid solution.
2. the method for fixed nitrogen in the water according to claim 1, it is characterized in that: the ground-electrode of described high pressure pulse discharge is in water, and forms discharge in water.
3. the method for fixed nitrogen in the water according to claim 1 is characterized in that: the ground-electrode of described high pressure pulse discharge is positioned at water surface top, forms gas-liquid mixed discharge.
4. the method for fixed nitrogen in the water according to claim 1 is characterized in that: described nitrogenous gas is a nitrogen.
5. the method for fixed nitrogen in the water according to claim 1 is characterized in that: described nitrogenous gas is an air.
6. the device of fixed nitrogen in the water, comprise reaction vessel, cooling system and power supply, it is characterized in that: the chamber in the described reaction vessel comprises main reaction chamber [1], be positioned at the air chamber [2] of main reaction chamber bottom, be positioned at the water coolant compartment [3] of main reaction chamber periphery, described air chamber is communicated with source of the gas, the air chamber top is provided with a plurality of aerating pores [6] and a plurality of pin shaped electric discharging electrodes to upper process [7], described water coolant compartment is communicated with cooling system, be provided with ground-electrode in the described main reaction chamber, described power supply is a high-voltage pulse power source, and its output is connected with ground-electrode with discharge electrode [7] respectively.
7. the device of fixed nitrogen in the water according to claim 6, it is characterized in that: described main reaction chamber [1] top is provided with lid [12], be provided with the grounding screw rod [11] that penetrates lid, ground-electrode in grounding screw rod lower end and the main reaction chamber is connected, the upper end is connected with the cathodic electricity of high-voltage pulse power source, has gas evolution mouth [13] on the lid.
8. the device of fixed nitrogen in the water according to claim 6 is characterized in that: the bottom that aerating pore stretches into main reaction chamber [1] is passed at the tip of described pin shaped electric discharging electrodes [7].
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AP3653A (en) | 2011-12-08 | 2016-04-02 | N2 Applied As | Reducing ammonia loss and odor from waste |
| CN107381723A (en) * | 2017-09-04 | 2017-11-24 | 南京大学 | A kind of sewage-treatment plant using more needle plate gas-liquid discharge in water plasmas |
| CN108101159A (en) * | 2018-01-15 | 2018-06-01 | 重庆工商大学 | A kind of high-pressure medium barrier discharge plasma wastewater treatment equipment |
| CN110327749A (en) * | 2019-07-18 | 2019-10-15 | 重庆工商大学 | A kind of method of low-temperature plasma degradation dimethylbenzene and synchronous fixed nitrogen |
| CN111362278A (en) * | 2020-02-21 | 2020-07-03 | 中国科学院电工研究所 | Device and method for preparing synthetic ammonia |
| CN116121779B (en) * | 2023-04-04 | 2023-07-14 | 北京化工大学 | Plasma-assisted electrocatalytic ammonia synthesis device and synthesis method thereof |
| CN116723622B (en) * | 2023-08-09 | 2023-10-27 | 北京航空航天大学 | Gas-liquid two-phase discharging device for improving nitrogen fertilizer yield |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100998A (en) * | 1987-03-02 | 1987-11-04 | 中国人民解放军第七零一八工厂 | The low-temp low-pressure method of nitric acid production through nitrogen fixation with air |
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2006
- 2006-07-11 CN CNB2006100863957A patent/CN100393612C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87100998A (en) * | 1987-03-02 | 1987-11-04 | 中国人民解放军第七零一八工厂 | The low-temp low-pressure method of nitric acid production through nitrogen fixation with air |
Non-Patent Citations (4)
| Title |
|---|
| 低温低压空气固氮制硝酸的研究. 喻忠普等.高等学校化学学报，第13卷第5期. 1992 |
| 低温低压空气固氮制硝酸的研究. 喻忠普等.高等学校化学学报，第13卷第5期. 1992 * |
| 强电离放电合成氨试验研究. 王燕等.大连海事大学学报，第28卷第2期. 2002 |
| 强电离放电合成氨试验研究. 王燕等.大连海事大学学报，第28卷第2期. 2002 * |
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