CN104729979A - High temperature water vapor oxidation experiment device capable of accurately controlling oxygen content - Google Patents

High temperature water vapor oxidation experiment device capable of accurately controlling oxygen content Download PDF

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Publication number
CN104729979A
CN104729979A CN201510141089.8A CN201510141089A CN104729979A CN 104729979 A CN104729979 A CN 104729979A CN 201510141089 A CN201510141089 A CN 201510141089A CN 104729979 A CN104729979 A CN 104729979A
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China
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high temperature
oxygen content
water
hand valve
steam generator
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CN201510141089.8A
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郦晓慧
陈锐
张锦文
奚杰峰
乔立捷
石岩
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Huadian Electric Power Research Institute Co Ltd
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Huadian Electric Power Research Institute Co Ltd
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Priority to CN201510141089.8A priority Critical patent/CN104729979A/en
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Abstract

The invention relates to a high temperature water vapor oxidation experiment device capable of accurately controlling oxygen content. The high temperature water vapor oxidation experiment device is structurally characterized by comprising a water vapor generation device, a high temperature pipe furnace, a quartz tube, a distilled water circulation loop, a water chemical parameter measurement pipeline, a control system, a vacuum pump, an exhaust device and a thermocouple. The high temperature water vapor oxidation experiment device has the control system, thus being capable of automatically and accurately carrying out dynamic control on the oxygen content and stably carrying out a water vapor oxidation experiment for a long time; therefore, the experiment efficiency is higher, the experimental data is closer to the actual working condition, and the device has higher guide value for actual operation.

Description

The high temperature water vapor oxidation experiment device of accurately controlling oxygen content
Technical field
The present invention relates to a kind of high temperature water vapor oxidation experiment device, particularly a kind of high temperature water vapor oxidation experiment device of accurately controlling oxygen content.
Background technology
As everyone knows, temperature is higher, and the utilization factor of heat energy is higher, and the coal quantity needed for unit generated energy is fewer.Therefore, under environmental protection and economy dual is ordered about, the single-machine capacity of fired power generating unit is more and more higher, and the temperature and pressure of operation also day by day improves.At present, overcritical and extra-supercritical unit becomes the main flow of China's thermal power industry gradually.In this kind of unit, heating surface tubes in boilers runs for a long time under the harsh operating mode of High Temperature High Pressure, often occur that steam side oxide skin large area is peeled off, the oxide skin of peeling off easily is piled up at bend part, thus cause superheater and reheater tube that the overheated pipe explosion accident caused because of the blocking of oxide skin bulk deposition locally occurs, have a strong impact on the security and economy that run in power station.Therefore, in the urgent need to carrying out high temperature water vapor oxidation simulated experiment, specifying high temperature water vapor oxidation mechanism and influence factor thereof, proposing reasonably prevention and mitigation strategy, and provide reference frame for the selection of high pressure high temperature turbosets.
At present, the steam oxidation simulated experiment carried out in the lab is roughly divided into two kinds: a kind of is the experiment of simulative power plant High Temperature High Pressure water-chemical regime in static high pressure pot, its shortcoming is in experimentation, water chemistry parameter in autoclave cannot be measured and control, and has larger gap with power plant actual condition; Another kind is the high-temperature oxydation experiment carried out in the water vapour of simulation flowing, and existing problem is that the oxygen content in circulating water steam cannot accurately control, and mostly adopts the mode of complete deoxygenation at present.But, under some special operation condition, in the feedwater of power plant's actual moving process, have the existence of a small amount of dissolved oxygen DO.
Summary of the invention
Technical matters to be solved by this invention be to provide a kind of reasonable in design, automatically, efficient, by testing sheet small sample thus the high temperature water vapor oxidation experiment device of the oxidation behavior of research material itself and the accurately controlling oxygen content of oxidation mechanism thereof.
It is as follows that the present invention solves the problems of the technologies described above adopted technical scheme:
The high temperature water vapor oxidation experiment device of accurately controlling oxygen content, comprises steam generator, high temperature process furnances, quartz ampoule, distilled water closed circuit, water chemistry parameter measurement pipeline, control system, vacuum pump, exhaust apparatus and thermopair,
Steam generator comprises automatic level controller, liquid level upper limit probe, liquid level lower limit probe, steam generator and heating arrangement, is provided with liquid level upper limit probe and liquid level lower limit probe in steam generator;
Distilled water closed circuit comprises water tank and water pump, distilled water closed circuit is also parallel with filtrator, distilled water closed circuit is connected with the top of water tank and bottom respectively, water tank is provided with inlet pipeline and discharge pipe line, water tank connects exhaust apparatus, steam generator, oxygen intake pipe and nitrogen/argon gas draft tube respectively, nitrogen/argon gas draft tube is divided into the first branch road and the second branch road, first branch road connects water tank, and the second branch road connects exhaust apparatus, steam generator, quartz ampoule respectively;
Water chemistry parameter measurement pipeline, comprise flowmeter, pH probe, dissolved oxygen probe and conductivity probe, one end of water chemistry parameter measurement pipeline connects water tank, and the other end connects water pump or filtrator;
Quartz ampoule is arranged among high temperature process furnances, and quartz ampoule connects exhaust apparatus, steam generator, thermopair respectively, and vacuum pump connects steam generator, quartz ampoule respectively;
Control system, comprise water chemistry parameter control system, automatic level controller, vapor (steam) temperature controller and tubular furnace temperature controller, water chemistry parameter control system is popped one's head in pH respectively, dissolved oxygen probe, conductivity probe, the first solenoid valve and the second solenoid valve are connected, and by computer program Process flowchart, automatic level controller is popped one's head in the liquid level upper limit respectively and liquid level lower limit is popped one's head in is connected, and tubular furnace temperature controller connects high temperature process furnances and thermopair respectively.
In the present invention, what inlet channel passed into is distilled water.
On the one hand, the present invention by arranging control system, can for a long time, stable, accurately automatically control oxygen content and carry out steam oxidation experiment, make related experiment result control to have higher guiding value to power plant's actual operating mode simultaneously; On the other hand, what the present invention adopted is sheet small sample, and the oxidation behavior of main research material itself and oxidation mechanism thereof, belong to micro-oxidation behavioral study.Therefore the present invention can under the prerequisite of accurate, stable regulation oxygen content, for sheet small sample, adopt quartz ampoule, carry out the oxidation mechanism of analysis of material itself from more basic and angle that is microcosmic, and then make experimental result of the present invention have more practical value.
The present invention by arranging distilled water closed circuit, thus carrying out distilled water controlling in the process of oxygen, avoiding the problem occurring dead angle, improve accuracy; The present invention by arranging filtrator between water tank and steam generator, avoid distilled water from water tank out after with impurity, the problem affecting service life of equipment, the accuracy of experimental result may be improve; The present invention can also realize in steam generator and high temperature process furnances segmentation, multiple deoxygenation, thus improves the accuracy of Control for Oxygen Content in experiment, improves the accuracy of experimental result.
As preferably, heating arrangement is the electric jacket that adjusts the temperature electronically, and vapor (steam) temperature controller is connected with the electric jacket that adjusts the temperature electronically.Its advantage is, compared to other heating arrangement, the electric jacket that adjusts the temperature electronically have quick heating, homogeneous temperature, temperature control more accurately, feature easily.
As preferably, water tank side is provided with water tank liquid level gauge.Its advantage is, can be understood the level condition of distilled water in water tank in real time, exactly, thus facilitate Control release process by water tank liquid level gauge.
As preferably, water tank is also provided with the first pipeline be communicated with air, and the first pipeline is provided with tensimeter and safety valve.Its advantage is, by tensimeter and safety valve, can control the pressure in water tank better, and according to Henry's law, under different pressure, the meltage of oxygen in distilled water is different; Can be discharged remaining distilled water in water tank after experiment terminates by discharge pipe line.
As preferably, the pipeline that the second branch road is connected with steam generator is provided with the 12 hand valve, and the pipeline that the second branch road is connected with quartz ampoule is provided with the 17 hand valve and the 16 hand valve successively.Its advantage is, by the control of valve, what can control inert gas passes into state, namely can realize passing into inert gas to steam generator and high temperature process furnances part on pretreatment, carries out deoxygenation.
As preferably, in quartz ampoule, be provided with air inlet coil pipe, be connected by frosted and high temperature resistant raw material band auxiliary seal between end socket with quartz ampoule.Its advantage is, because the temperature in the temperature and high temperature process furnances of steam generator water vapour out has relatively large deviation, it is temperature required that air inlet coil pipe can make the water vapour flowed through be heated to experiment further; By the auxiliary seal of high temperature resistant raw material band, improve the sealing property of end socket and quartz ampoule junction further.
As preferably, steam generator is connected with water pump or filtrator by the 3rd solenoid valve, the 3rd solenoid valve connection automatic level controller.Its advantage is, is controlled the state of the 3rd solenoid valve by automatic level controller, thus whether control distilled water enters steam generator, and the amount of distilled water, thus improves automatic controlling level and precision; And the 3rd solenoid valve can be closed in experimentation, the oxygen content of distilled water in adjustment water tank, then open the 3rd solenoid valve and carry out oxidation experiment, make the controllability of testing higher.
As preferably, distilled water closed circuit is provided with the 8th hand valve, and filtrator connects the 6th hand valve and the 7th hand valve respectively, and in parallel with the 8th hand valve.Its advantage is, by the setting of valve, when the distilled water in water tank contains graininess impurity, selects to filter it, thus ensures the accuracy of experiment and the serviceable life of extension device.
As preferably, the range of control of oxygen content is for being less than between 10ppb to 8ppm; The operating temperature range of high temperature process furnances (16) is 600 degrees Celsius to 900 degrees Celsius, and the temperature control precision in quartz ampoule (19) is ± 1 degree Celsius; The maximum operating temperature of electric jacket (14) of adjusting the temperature electronically is 200 degrees Celsius.Its advantage is, because the present invention can realize automatic control, and therefore can high precision and the parameter such as temperature, oxygen content of Control release on a large scale.
The present invention compared with the existing technology has the following advantages and effect:
1, the present invention is by the dissolved oxygen content in distilled water in real―time precision measurment, record, display and control water tank, and then controls the oxygen content in water vapour, make experimental situation and power plant's actual condition more close, experimental result has more reference value.
2, present invention achieves the segmentation in steam generator, quartz ampoule and associated pipe, multiple deoxygenation, ensure that accuracy and the stability of Control for Oxygen Content in system.
3, present invention achieves the automatic control of steam generator water level, can for a long time, stable carry out steam oxidation experiment, conventional efficient is high.
4, the present invention is by the water chemistry parameter of real time record, bond material oxidizing process, can further clear and definite oxygen content on the impact of material in high-temperature water vapor, for Water of Power Plant Chemical Control provides reference frame.
5, in the present invention, dissolved oxygen DO control system, water vapour generation systems and high temperature water vapor oxidation system are relatively independent, and pipeline connects and runs control conveniently, and is convenient to the follow-up maintenance to each several part and upgrading.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is structural representation of the present invention.
Label declaration:
1, water tank 2, water pump 3, filtrator
4, tensimeter 5, safety valve 6, flowmeter
7, pH probe 8, dissolved oxygen probe 9, conductivity probe
10, automatic level controller 11, liquid level upper limit probe 12, liquid level lower limit probe
13, steam generator 14, adjust the temperature electronically electric jacket 15, vacuum pump
16, high temperature process furnances 17, end socket 18, sample
19, quartz ampoule 20, thermopair 21, exhaust apparatus
22, water tank liquid level gauge 23, reduction valve 101, first hand valve
102, the second hand valve 103, the 3rd hand valve 104, the 4th hand valve
105, the 5th hand valve 106, the 6th hand valve 107, the 7th hand valve
108, the 8th hand valve 109, the 9th hand valve 110, the tenth hand valve
111, the 11 hand valve the 112, the 12 hand valve the 113, the 13 hand valve
114, the 14 hand valve the 115, the 15 hand valve the 116, the 16 hand valve
117, the 17 hand valve the 118, the 18 hand valve 201, first solenoid valve
202, the second solenoid valve 203, the 3rd solenoid valve 91, water inlet pipe
92, oxygen intake pipe 93, nitrogen/argon gas draft tube 931, first branch road
932, the second branch road 94, distilled water closed circuit 95, water chemistry parameter measurement pipeline
96, discharge pipe line 97, first pipeline
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, and following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1:
As shown in Figure 1, the present embodiment is by mainly comprising: water tank 1, water pump 2, filtrator 3, flowmeter 6, pH probe 7, dissolved oxygen probe 8, conductivity probe 9, automatic level controller 10, liquid level upper limit probe 11, liquid level lower limit probe 12, steam generator 13, the electric jacket 14 that adjusts the temperature electronically, vacuum pump 15, high temperature process furnances 16, end socket 17, sample 18, quartz ampoule 19, thermopair 20, exhaust apparatus 21, water tank liquid level gauge 22, reduction valve 23, and concrete structure is as follows:
Water tank 1 is connected with two draft tube, and namely oxygen intake pipe 92 and nitrogen/argon gas draft tube 93, can pass into oxygen and nitrogen/argon gas respectively.Nitrogen/argon gas draft tube 93 is divided into two branch roads, i.e. the first branch road 931 and the second branch road 932.First branch road 931 is communicated with water tank 1, and the first branch road 931 is provided with the first solenoid valve 201 and retaining valve.Second branch road 932 is communicated with exhaust apparatus 21, the second branch road 932 is provided with successively the first hand valve 101, retaining valve, the 17 hand valve the 117 and the 18 hand valve 118.Between retaining valve and the 17 hand valve 117, separate a road be connected with the water inlet of steam generator 13, the pipeline be connected with steam generator 13 is provided with the 12 hand valve 112; Between the 17 hand valve the 117 and the 18 hand valve 118, separate a road be connected with the venthole of quartz ampoule 19, the pipeline be connected with the venthole of quartz ampoule 19 is provided with the 16 hand valve 116.
The pipeline that oxygen intake pipe 92 is communicated with water tank 1 is provided with the second solenoid valve 202 and retaining valve, and retaining valve can prevent gas backflow in water tank 1.
Water tank 1 is communicated with air by the first pipeline 97, and the first pipeline 97 is provided with tensimeter 4 and safety valve 5, and the air pressure in water tank 1 reads by the tensimeter 4 be arranged on above water tank 1.Water tank 1 is also communicated with exhaust apparatus 21, and this connecting pipeline is provided with the 3rd hand valve 103 and reduction valve 23, utilizes reduction valve 23 can to control the air pressure in water tank 1.According to Henry's law, by oxygen content numerical value in distilled water temperature estimation solution in partial pressure and water tank 1, thus the setting of pressure in water tank 1 can be instructed.
The purpose that exhaust apparatus 21 is set be by degasification of the present invention after gas and water vapour after experiment discharge.Two tubes in exhaust apparatus 21 reaches below liquid level, exactly in order to prevent air suck-back from entering in experimental provision.
Water tank 1 is also provided with water inlet pipe 91, and water inlet pipe 91 is provided with the second hand valve 102, for injecting distilled water in water tank 1.
Be provided with distilled water closed circuit 94 in the present invention, this distilled water closed circuit 94 is followed successively by: water tank 1, the 5th hand valve 105, water pump 2, the 8th hand valve 108, the 9th hand valve 109, retaining valve.8th hand valve 108 is parallel with a pipeline, and this pipeline is provided with the 6th hand valve 106, filtrator 3, the 7th hand valve 107.Filtrator 3 can elimination large granular impurity, also can close the 6th hand valve 106, the 7th hand valve 107 that are arranged on before and after filtrator 3, opening the 8th hand valve 108 when not having large granular impurity in the solution in distilled water closed circuit 94.
Pipeline between 5th hand valve 105 and water tank 1 separates a road, i.e. discharge pipe line 96, which is provided with the 4th hand valve 104.
Water chemistry parameter measurement pipeline 95 is also provided with in the present invention, it is connected in parallel on the pipeline of the 9th hand valve 109 and retaining valve, and water chemistry parameter measurement pipeline 95 is provided with the tenth hand valve 110, flowmeter 6, pH probe 7, dissolved oxygen probe 8, conductivity probe 9 and retaining valve.
Can oxygen content in Real-Time Monitoring water tank 1 by dissolved oxygen probe 8, thus realize the real-time adjustment of oxygen content and control for a long time, stably, pH probe 7 and the effect of conductivity probe 9 are exactly the character of distilled water in reflection water tank 1, and its benefit is the experimental data contrast be convenient under different condition.
8th hand valve 108 is also connected the water inlet of steam generator 13 with the water delivering orifice of filtrator 3 by pipeline, the pipeline that the water delivering orifice of this filtrator 3 is connected with steam generator 13 is disposed with: the 11 hand valve 111, the 3rd solenoid valve 203, retaining valve, threeway.
Be provided with liquid level upper limit probe 11 and liquid level lower limit probe 12 in steam generator 13, and be connected with automatic level controller 10 by wire.Automatic level controller 10 controls the switch of the 3rd solenoid valve 203.
Steam generator 13 is heated by the electric jacket 14 that adjusts the temperature electronically, and the electric jacket 14 that adjusts the temperature electronically is connected with vapor (steam) temperature controller, and controls by it.Compared to other heating arrangement, adjust the temperature electronically electric jacket 14 quick heating, homogeneous temperature, temperature control more accurately, feature easily.
The outlet of steam generator 13 is communicated with the quartz ampoule 19 be arranged in high temperature process furnances 16 by pipeline, and the pipeline that the outlet of this steam generator 13 is communicated with quartz ampoule 19 is provided with the 13 hand valve the 113 and the 15 hand valve 115.Wherein, separate a road between 13 hand valve the 113 and the 15 hand valve 115 to be connected with vacuum pump 15, this pipeline is provided with the 14 hand valve 114, namely vacuum pump 15 is communicated with quartz ampoule 19 with steam generator 13 respectively, on pretreatment to the deoxygenation of bleeding in steam generator 13, quartz ampoule 19 and associated pipe.
Quartz ampoule 19 is arranged in high temperature process furnances 16, is provided with air inlet coil pipe in it, is connected between end socket 17 with quartz ampoule 19 by frosted and high temperature resistant raw material band auxiliary seal.Because the temperature in steam generator 13 steam temperature out and high temperature process furnances 16 has relatively large deviation, air inlet coil pipe makes the water vapour flowed through be heated to experimental temperature further.By the auxiliary seal of high temperature resistant raw material band, improve the sealing property of end socket 17 and quartz ampoule 19 junction further.
In the present embodiment, in quartz ampoule 19, be also provided with thermopair 20 and sample 18.Temperature signal, for measuring the experimental temperature in quartz ampoule 19, is transferred to tubular furnace temperature controller by thermopair 20, and controls the heating power of high temperature process furnances 16 by tubular furnace temperature controller.The temperature being measurement gained thermopair 20 benefit be arranged in quartz ampoule 19 is exactly experimental temperature, avoids and thermopair 20 is arranged on the measuring tempeature and actual experiment temperature deviation that cause in high temperature process furnances 16.
When the present invention works, first the water chemistry parameter in water tank 1 is adjusted to requirement of experiment.Then, open the 11 hand valve 111 successively, open fluid level controller 10, adjust the temperature electronically electric jacket 14 and high temperature process furnances 16.The water vapour produced in steam generator 13 passes in quartz ampoule 19 with pipeline, and contacts with sample 18 after heating further, finally enters in exhaust apparatus 21.Experimental temperature in this steam oxidation experimental provision and the oxygen content in water vapour accurately control.
Distilled water volume in water tank 1 reads by water tank liquid level gauge 22.Water tank liquid level gauge 22 adopts quartz glass to make.
Steam generator 13 in the present invention, quartz ampoule 19 and associated pipe, by valve regulated, realize passing into nitrogen or argon gas and vacuum pump 15 and to bleed two kinds of mode deoxygenations, and vacuum pump 15 can be bled to steam generator 13 and quartz ampoule 19 separately.
In the present invention, control system comprises water chemistry parameter control system, automatic level controller 10, vapor (steam) temperature controller and tubular furnace temperature controller, water chemistry parameter control system pops one's head in 7 respectively with pH, dissolved oxygen probe 8, conductivity probe 9, first solenoid valve 201 and the second solenoid valve 202 are connected, and by computer program Process flowchart; Automatic level controller 10 pop one's head in the liquid level upper limit respectively 11 and liquid level lower limit pop one's head in and 12 to be connected, tubular furnace temperature controller connects high temperature process furnances 16 and thermopair 20 respectively.
Control mode of the present invention is as follows:
(1) control system controls the open and close of water pump 2;
(2) pH probe 7, dissolved oxygen probe 8, conductivity probe 9 input measuring the current signal obtained in water chemistry parameter control system, and input in computing machine, and carry out on computers showing and record after converting digital signal to;
The open and close of (3) the 3rd solenoid valves 203 can manually control, and also automatically can be controlled by fluid level controller 10;
(4) temperature signal that thermopair 20 records is input in tubular furnace temperature controller, and tubular furnace temperature controller controls the heating power of high temperature process furnances 16;
(5) current signal is reached the input end of control system by dissolved oxygen probe 8; The output terminal of control system controls nitrogen/argon gas first solenoid valve 201 and oxygen second solenoid valve 202; Computer controlled automatic program controls the switching value size of nitrogen/argon gas first solenoid valve 201 or oxygen second solenoid valve 202 respectively according to the difference of the dissolved oxygen content preset in the dissolved oxygen content of actual measurement and system.
The high temperature water vapor oxidation experiment device operation part of accurately controlling oxygen content of the present invention can be divided into two parts, and Part I is setting and the adjustment member of systematic parameter, and Part II is experimental implementation part.As follows respectively:
Part I: the setting and adjustment part (in default system, each valve is initial is closed condition) of systematic parameter
(1) open the second hand valve 102, inject distilled water by Miniature water-pumping pump in water tank 1, volume is between 1/2 to 2/3 of water tank 1 volume;
(2) close the second hand valve 102, and utilize cutting ferrule to receive nitrogen/argon gas bottle in the import of the second hand valve 102, slowly open air valve on gas cylinder until when the top hole pressure registration of air valve is 0.15MPa, stop the adjustment of air valve;
(3) slowly open the second hand valve 102, according to the size of the tensimeter 4 reading regulation safety valve 5 that water tank 1 is installed, then close the second hand valve 102;
(4) the air valve export pipeline on nitrogen/argon gas bottle is connected to the co-portal place of the first hand valve 101 and the first solenoid valve 201 by cutting ferrule;
(5) close the first hand valve 101, open the 3rd hand valve 103; Experimentally requirement, in conjunction with tensimeter 4 registration, slowly regulates reduction valve 23;
(6) the 5th hand valve 105, the 6th hand valve 106, the 7th hand valve 107, the 9th hand valve 109 and the tenth hand valve 110 is opened successively;
(7) device for opening general supply, is energized to control system each several part;
(8) adjust liquid level upper limit probe 11 and the position of liquid level lower limit probe 12 in steam generator 13, and be connected with automatic level controller 10, the mode of operation of setting automatic level controller 10;
(9) open the 11 hand valve 111 and manually opened 3rd solenoid valve 203, distilled water is injected steam generator 13, make water level between liquid level upper limit probe 11 and liquid level lower limit probe 12;
(10) thermopair 20 is arranged in quartz ampoule 19, and the temperature of actual measurement is transferred in the temperature controller of high temperature process furnances 16; According to the heat characteristic of system, Self-tuning System pattern is adopted to draw rational heating curves.
Part II: experimental implementation part (in default system, each valve is initial is closed condition)
(1) open the second hand valve the 102, three hand valve 103 and reduction valve 23, in water tank 1, inject distilled water, the distilled water volume of injection is between 1/2 to 2/3 of water tank 1 volume;
(2) sample 18 is ready to put into quartz ampoule 19, with end socket 17, quartz ampoule 19 is sealed, and tangle with high temperature resistant raw material band is auxiliary;
(3) if having large granular impurity in the distilled water of circulation, select to open the 6th hand valve 106 and the 7th hand valve 107, close the 8th hand valve 108; If there is no large granular impurity in the distilled water of circulation, select closedown the 6th hand valve 106 and the 7th hand valve 107, open the 8th hand valve 108;
(4) the 5th hand valve 105, the 9th hand valve 109 and the tenth hand valve 110 is opened successively;
(5) chemical parameters adjustment portion of fetching boiling water general supply, to the energising of this part all parts, and runs automatic control program, program interface sets the parameter such as dissolved oxygen content and system operation time;
(6) open water pump 2 operational system a period of time, in conjunction with automatic control system, make the dissolved oxygen content of distilled water in water tank 1 reach experiment setting value;
(7) open the 18 hand valve the 118, the 16 hand valve the 116, the 15 hand valve the 115, the 13 hand valve the 113, the 12 hand valve 112 and the first hand valve 101 successively, pass into nitrogen or argon gas deoxygenation in steam generator 13 and quartz ampoule 19;
(8) close the 12 hand valve the 112, the 16 hand valve the 116 and the 17 hand valve 117 successively, open the 14 hand valve 114 and vacuum pump 15;
(9) close the 14 hand valve 114, vacuum pump 15, open the 12 hand valve 112;
(10) close the first hand valve the 101, the 12 hand valve 112 successively, open the 16 hand valve 116;
(11) manual unlocking the 3rd solenoid valve 203 also slowly opens the 11 hand valve 111, makes distilled water slowly inject steam generator 13;
(12) link heating power, automatic level controller 10, the liquid level upper limit probe 11 adjusting the electric jacket 14 that adjusts the temperature electronically, and liquid level lower limit probe the 12, three solenoid valve the 203 and the 11 hand valve 111, makes steam generator 13 go out vapour and stablize;
(13) open the heating power supply switch of high temperature process furnances 16, and with tubular furnace temperature controller, its heating power is controlled;
(14), after experiment terminates, the heater switch of high temperature process furnances 16, the heater switch of the electric jacket 14 that adjusts the temperature electronically, the switch of automatic level controller 10 and the 11 hand valve 111 is closed successively;
(15) control system and each valve of dissolved oxygen content adjustment portion is closed;
(16) after quartz ampoule 19 is cooled to room temperature, sample 18 is taken out and carries out follow-up experimental analysis.
In the present invention, oxygen content regulates by carrying out automatic control and adjustment realization in water tank 1.After oxygen content is adjusted to the scope of requirement of experiment, first pass in steam generator 13, after heating becomes water vapour, then pass in the quartz ampoule 19 in high temperature process furnances 16.
The oxygen content related in the present invention regulates and only completes in water tank 1, can not carry out oxygen content adjustment, but carry out deoxygenation in equipment and pipeline by passing into nitrogen/argon gas on pretreatment in steam generator 13 and high temperature process furnances 16.
Can ventilation deoxygenation be carried out separately or simultaneously or vacuumize deoxygenation in quartz ampoule 19 in steam generator 13 and high temperature process furnances 16.
The control of oxygen content needs the data that record according to oxygen content probe 8 and setting value to contrast, and is then undertaken adjusting and controlling by the computer program of designed, designed.Different oxygen content setting ranges, the parameter in computer-controlled program is also different.In general, the oxygen content in water tank 1 is minimum can at below 10ppb; Setting oxygen content is when 100ppb, and reality can control at 80 to 120ppb, ± 20ppb; Setting oxygen content is when 2000ppb, and reality can control at 1980 to 2020ppb, ± 20ppb.
In sum, the present invention compared with the existing technology has the following advantages:
1, the present invention adopts sheet small sample 18, and the oxidation behavior of main research material itself and oxidation mechanism thereof, belong to micro-oxidation behavioral study, and achievement in research has darker purpose and purposes widely, has higher directive significance to practical operation.
2, because the present invention can realize automatically being controlled the oxygen content in experimentation and temperature by a complete control device, comprise the parts such as feedback, control and record, and automaticity and precision are all relatively high, accurate, long-time, stable control can be carried out to the oxygen content of water vapour in the present invention, there is higher conventional efficient, work condition environment in more realistic operation simultaneously, experimental result has higher reference and directive significance to practical operation.
3, oxygen content of the present invention range of control be 10ppb to 8ppm, this range of control is far wide in prior art, and scope of experiment is more extensive, and experimental result has more cogency.
4, the present invention is while measurement oxygen content, is also provided with pH probe 7 and conductivity probe 9, the more enough character more fully reflected for generation of the distilled water of water vapour in the present invention.
In addition, it should be noted that, the specific embodiment described in this instructions, the shape, institute's title of being named etc. of its parts and components can be different.All equivalences of doing according to structure, feature and the principle described in inventional idea of the present invention or simple change, be included in the protection domain of patent of the present invention.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.

Claims (9)

1. the high temperature water vapor oxidation experiment device of an accurately controlling oxygen content, comprise steam generator, high temperature process furnances (16) and quartz ampoule (19), it is characterized in that: also comprise distilled water closed circuit (94), water chemistry parameter measurement pipeline (95), control system, vacuum pump (15), exhaust apparatus (21) and thermopair (20)
Described steam generator comprises automatic level controller (10), liquid level upper limit probe (11), liquid level lower limit probe (12), steam generator (13) and heating arrangement, is provided with liquid level upper limit probe (11) and liquid level lower limit probe (12) in described steam generator (13);
Described distilled water closed circuit (94) comprises water tank (1) and water pump (2), described distilled water closed circuit (94) is also parallel with filtrator (3), described distilled water closed circuit (94) is connected with the top of described water tank (1) and bottom respectively, described water tank (1) is provided with inlet pipeline (91) and discharge pipe line (96), described water tank (1) connects described exhaust apparatus (21) respectively, steam generator (13), oxygen intake pipe (92) and nitrogen/argon gas draft tube (93), described nitrogen/argon gas draft tube (93) is divided into the first branch road (931) and the second branch road (932), described first branch road (931) connects described water tank (1), described second branch road (932) connects described exhaust apparatus (21) respectively, steam generator (13), quartz ampoule (19),
Described water chemistry parameter measurement pipeline (95), comprise flowmeter (6), pH probe (7), dissolved oxygen probe (8) and conductivity probe (9), one end of described water chemistry parameter measurement pipeline (95) connects described water tank (1), and the other end connects described water pump (2) or filtrator (3);
Described quartz ampoule (19) is arranged among high temperature process furnances (16), described quartz ampoule (19) connects described exhaust apparatus (21), steam generator (13), thermopair (20) respectively, and described vacuum pump (15) connects described steam generator (13), quartz ampoule (19) respectively;
Control system, comprise water chemistry parameter control system, automatic level controller (10), vapor (steam) temperature controller and tubular furnace temperature controller, described water chemistry parameter control system pops one's head in (7) with pH respectively, dissolved oxygen probe (8), conductivity probe (9), first solenoid valve (201) is connected with the second solenoid valve (202), and by computer program Process flowchart, described automatic level controller (10) is popped one's head in (11) with the described liquid level upper limit respectively and liquid level lower limit is popped one's head in, and (12) are connected, described tubular furnace temperature controller connects described high temperature process furnances (16) and thermopair (20) respectively.
2. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 1, it is characterized in that: described heating arrangement is connected with the electric jacket that adjusts the temperature electronically (14) for the electric jacket that adjusts the temperature electronically (14), described vapor (steam) temperature controller.
3. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 1, is characterized in that: described water tank (1) side is provided with water tank liquid level gauge (22).
4. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 3, it is characterized in that: described water tank (1) is also provided with the first pipeline (97) be communicated with air, described first pipeline (97) is provided with tensimeter (4) and safety valve (5).
5. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 1, it is characterized in that: the pipeline that described the second branch road (932) is connected with steam generator (13) is provided with the 12 hand valve (112), the pipeline that described the second branch road (932) is connected with quartz ampoule (19) is provided with the 17 hand valve (117) and the 16 hand valve (116) successively.
6. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 1, it is characterized in that: be provided with air inlet coil pipe in described quartz ampoule (19), end socket (17) is tightly connected by high temperature resistant raw material band and described quartz ampoule (19).
7. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 1, it is characterized in that: described steam generator (13) is connected with water pump (2) or filtrator (3) by the 3rd solenoid valve (203), the 3rd described solenoid valve (203) connects automatic level controller (10).
8. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 1, it is characterized in that: described distilled water closed circuit (94) is provided with the 8th hand valve (108), described filtrator (3) connects the 6th hand valve (106) and the 7th hand valve (107) respectively, and in parallel with the 8th hand valve (108).
9. the high temperature water vapor oxidation experiment device of accurately controlling oxygen content according to claim 1, is characterized in that: the range of control of oxygen content is for being less than between 10ppb to 8ppm; The operating temperature range of described high temperature process furnances (16) is 600 degrees Celsius to 900 degrees Celsius, and the temperature control precision in described quartz ampoule (19) is ± 1 degree Celsius; The maximum operating temperature of the described electric jacket that adjusts the temperature electronically (14) is 200 degrees Celsius.
CN201510141089.8A 2015-03-27 2015-03-27 High temperature water vapor oxidation experiment device capable of accurately controlling oxygen content Pending CN104729979A (en)

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