CN103064437A - Device and method for controlling dissolved oxygen in reaction container - Google Patents

Device and method for controlling dissolved oxygen in reaction container Download PDF

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Publication number
CN103064437A
CN103064437A CN2012105943953A CN201210594395A CN103064437A CN 103064437 A CN103064437 A CN 103064437A CN 2012105943953 A CN2012105943953 A CN 2012105943953A CN 201210594395 A CN201210594395 A CN 201210594395A CN 103064437 A CN103064437 A CN 103064437A
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valve
solution
solution cylinder
dissolved oxygen
inert gas
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CN103064437B (en
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卢国华
朱志平
苏伟
周艺
陈天生
陆海伟
马存仁
刘世念
付强
钱艺华
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Changsha University of Science and Technology
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Changsha University of Science and Technology
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Abstract

The invention discloses a device for controlling dissolved oxygen in a reaction container. The device comprises a solution cylinder provided with a top cover, and further comprises a high pressure reaction kettle provided with a liquid phase sampling valve and a gas pulse sampling valve, wherein the gas pulse sampling valve is connected to a gas storage bottle used for storing inert gases; a dissolved oxygen probe, an agitating vane controlled by a stirrer, and a gas inlet pipe used for being connected with the gas storage bottle for storing the inert gases are arranged in the solution cylinder, and both the dissolved oxygen probe and the stirrer are connected to the interior of a controller; the bottom of the solution cylinder is connected with the liquid phase sampling valve through a three-way valve; and a pressure-limiting valve, a safety valve, a liquid inlet valve and a vent valve are arranged on the outer surface of the top cover, the pressure-limiting valve, the safety valve, the liquid inlet valve and the vent valve are communicated with the interior of the solution cylinder, the top of the liquid inlet valve is higher than that of the vent valve, and an inlet valve is arranged on the gas inlet pipe. The invention further discloses a method for controlling the dissolved oxygen in the reaction container.

Description

The device and method of control dissolved oxygen DO in reaction vessel
Technical field
The present invention relates to the technical field of dissolved oxygen DO, particularly relate to a kind of device and method of in reaction vessel, controlling dissolved oxygen DO.
Background technology
Existing in the heat power equipments such as Industrial Boiler, station boiler and reactor, the working environment of the high-temperature high pressure water of hypoxemia or steam normally.In the laboratory, designed polytype high-temperature high-pressure reaction kettle under this high-temperature and high-pressure conditions in order to simulate.Basic demand to autoclave is good leak tightness, can not the seepage liquids and gases; Autoclave inner-wall therefore must be corrosion-resistant because being in the same corrosion environment with sample; Enough intensity should be arranged, bear long-term High Pressure; Be experimental safe and satisfy the kinds of experiments requirement, should set up the device of some necessity, such as the temperature and pressure control device, safety feature and electrochemical measurement interface etc.
Yet, the concentration of solute can't be identical with the operating condition of actual heat power equipment in some pacing itemss that only can guarantee high-temperature high-pressure reaction kettle and the solution, particularly in the experiment of reality and research process, be difficult to the dissolved oxygen content in the water carry out effectively, accurately control, to such an extent as to owing to can't reach the oxygen content condition of determining concentration and cause and test and the result of study distortion.Even pass into a large amount of inert gases in reaction vessel, control reaction vessel and reaction solution are also very difficult at low oxygen content.In actual production, for the boiler of different parameters, its Control for Oxygen Content index is different.For example, regulation among the GB/T1576-2008 " Industrial Boiler water quality ", nominal steam pressure is less than or equal to the boiler of 1MPa and greater than the boiler of 1.0MPa less than or equal to 1.6MPa feedwater employing softening water, and the feedwater dissolved oxygen content is less than or equal to 0.1mg/L; Less than the boiler of 3.8MPa and greater than the boiler of 1.0MPa less than or equal to 1.6MPa feedwater employing demineralized water, the feedwater Control for Oxygen Content is less than or equal to 0.05mg/L greater than 1.6MPa for nominal steam pressure.The dum boiler feedwater dissolved oxygen content of regulation 3.8-5.8MPa is less than or equal to 15 μ g/L in GB/T12145-2008 " thermal power generation unit and apparatus of steam power plants Water Vapor Quality ", and pressure is controlled less than or equal to 7 μ g/L greater than the dum boiler feedwater dissolved oxygen DO of 5.9MPa; It is 30-150 μ g/L that oxygenation is processed dissolved oxygen DO control content.In nuclear power station, the dissolved oxygen content in the various waters also has strict control index.In a lot of experiments and research, because therefore the oxygen content in the very difficult control solution accomplishes that the simulated hypoxia high temperature and high pressure condition is identical with actual condition or close equally very difficult.
At present, in the simulated experiment of carrying out in high-temperature high-pressure reaction kettle and other reaction vessels and the research, the control for oxygen content in the solution is the N that passes into certain flow by reaction solution in autoclave or reaction vessel usually 2Or other inert gas carries out the deoxygenation operation to solution.But oxygen content is subject to the impact of temperature in the aqueous solution, and saturated oxygen content is different under the different temperatures, and more low oxygen content is also higher for general temperature.During logical inert gas deoxygenation, also to be subject to treating the impact of the many factors such as liquor capacity, charge flow rate, system pressure of deoxygenation, simple pass through the control charge flow rate and can't guarantee that the oxygen content for the treatment of deoxygenation solution reaches experiment and research requirement.Autoclave or other reaction vessels are after adding solution, because the liquid level top still is air in the reaction vessel.The volume fraction of oxygen is 21% in the meter air, the oxygen molal weight is 32g/mol, molar volume of gas is 22.4L/mol, then contain oxygen 100mL * 21% * 32g/mol/(22400mL/mol)=0.03g=30mg in the 100mL air, with 100mL air 9900mL inert gas dilution, oxygen concentration then is 0.3mg/100mL gas.If when needing to guarantee that oxygen level is less than or equal to 30 μ g/100mL in the gas, need 99900mL(99.9L) inert gas, so the inert gas consumption is very large, and can not accurately control the oxygen content of solution in the reaction vessel.Partial reaction container (such as autoclave) is high temperature pressure vessel, installs high-temperature digestion oxygen electrode somewhat expensive additional, and also is difficult to install additional in narrow and small reaction compartment inside.In addition, install the generation stress that the high-temperature digestion oxygen electrode also may cause metal material additional, affect its serviceable life.
For experiment or the research of dissolved oxygen content in other control solution, also be first solution to be placed reaction vessel, by in reaction vessel, passing into inert gas solution is carried out deoxygenation again.Although such Deoxidization method can be removed oxygen a large amount of in the solution, but same because there is certain space in reaction vessel top, cause after the solution deoxygenation finishes, the remaining oxygen in solution top continues soluble in water, and this is not so that oxygen removal process is reduced to minimum level with effect of oxygen completely.And for the less reaction vessel of volume, more difficult control.If when oxygen has a significant impact for whole result of study, still cause data distortion.
Therefore, uneconomical and insecure (when oxygen content was reduced to setting in the solution, the impact of sheaf space was still ignored on the solution) by in reaction vessel, directly passing into inert gas and in high-temperature high-pressure reaction kettle, installing the high-temperature digestion oxygen electrode additional with solution oxygen content in the accurate control high-temperature high-pressure reaction kettle.Directly in the reaction vessels such as autoclave, pass into the oxygen content that inert gas can not be controlled solution accurately.
Summary of the invention
Based on this, for existing issue, be necessary to propose a kind of device and method of in reaction vessel, controlling dissolved oxygen DO, can control accurately the oxygen content of solution.
For solving the problems of the technologies described above, the invention provides a kind of device of in reaction vessel, controlling dissolved oxygen DO, comprise the solution cylinder with top cover, also comprise the autoclave with liquid phase sample valve and gas phase sample valve, described gas phase sample valve is connected to for the gas bomb that stores inert gas, be provided with dissolved oxygen probe in the described solution cylinder, stirring vane and the draft tube that is connected connecting the gas bomb that stores inert gas by stirrer control, described dissolved oxygen probe and described stirrer all connect into controller, the bottom of described solution cylinder is connected with the liquid phase sample valve by T-valve, the outside surface of described top cover is provided with the pressure limiting valve that communicates with solution cylinder inside, safety valve, liquid feed valve and vent valve, the top of described liquid feed valve is higher than the top of described vent valve, and described draft tube is provided with gas admittance valve.
In the technical program, pressure limiting valve places the top cover outside surface to keep cylinder pressure constant; Gas admittance valve places top cover top and connects up and down draft tube, and top cover top draft tube links to each other with source of the gas, and the bottom draft tube places in the solution cylinder, makes air inlet pass into the solution bottom; Dissolved oxygen probe places the top cover bottom, and dissolved oxygen probe placed solution after top cover was installed on the solution cylinder; Stirrer is installed on the top cover, in order to guarantee the even of solution; Controller is connected with dissolved oxygen probe and stirrer, to show and to record the numerical value of dissolved oxygen DO and control stirring rate; Safety valve guaranteed solution cylinder pressure safety when pressure limiting valve lost efficacy; Liquid feed valve is in order to dosing in cylinder; Vent valve places top cover, makes cylinder pressure identical with atmospheric pressure when it is opened.Pressure limiting valve discharges gas to guarantee the constant pressure in the solution cylinder in the excessive situation of the rear pressure of solution cylinder sealing, prevent that simultaneously air from entering in the solution cylinder; Gas admittance valve is used for controlling inert gas and enters in the solution cylinder; Dissolved oxygen probe places solution to measure the solution oxygen content; Stirrer in order to guarantee the homogeneity of solution, reaches the purpose of even deoxygenation when the ventilation deoxygenation; T-valve is used and is derived the solution of deoxygenation, and can carry out sampling and the discharge opeing of an interior liquid; Controller is used for showing and the record dissolved oxygen content observe whether oxygen content reaches requirement and adjust the stirrer rotational speed in the solution; When safety valve is used for the pressure limiting valve inefficacy, guarantee solution cylinder safety; Liquid feed valve is used for adding medicament in the solution cylinder; Vent valve guarantees that when dosing the solution cylinder pressure equals atmospheric pressure, and is used for Exhaust Gas.
In a preferred embodiment, described top cover is sealedly attached to the top of described solution cylinder by packing washer.Purpose is the impermeability that guarantees whole system.
In a preferred embodiment, described solution cylinder is the graduated container of tool.Purpose is to limit the volume that imports solution.
In a preferred embodiment, described safety valve is spring safety valve.Purpose is to guarantee that safety valve can use well.
In a preferred embodiment, described gas admittance valve is located at the top of described top cover.Purpose is to guarantee smoothly operation and adjust gas admittance valve.
In a preferred embodiment, described controller is provided with display device.Purpose is the numerical value of being convenient to observe control.
In a preferred embodiment, the first connector of described T-valve is connected in the bottom sides of described solution cylinder, and the second connector connects described liquid phase sample valve, the conduit that the joint among three members connection communicates with atmosphere.Purpose is that the assurance T-valve can be realized goal of the invention smoothly.
For solving the problems of the technologies described above, the present invention also provides a kind of method of controlling dissolved oxygen DO in reaction vessel, may further comprise the steps:
A. in autoclave, fill with water or other liquid, again the water in the autoclave or liquid are discharged with inert gas, make to be oxygen-free environment in the autoclave;
B. will treat that the reaction solution of deoxygenation injects the solution cylinder of anaerobic, and pass into inert gas in the solution cylinder and keep in the solution cylinder positive pressure environment that reaction solution is carried out deoxygenation, and control it and reach setting value and namely finish deoxygenation;
C. the reaction solution with deoxygenation passes in the autoclave under the environment that does not contact oxygen.
In a preferred embodiment, step a may further comprise the steps:
In the solution cylinder, be full of water or other liquid, pass into inert gas in the solution cylinder again water or liquid are pressed out in the autoclave kettle;
After in the autoclave kettle, filling with water or other liquid, stop in the solution cylinder, passing into inert gas;
Open T-valve the autoclave kettle is linked to each other with atmosphere, pass into inert gas in the autoclave kettle water or other liquid in the autoclave kettle are discharged, until be the inert gas space of anaerobic in the autoclave kettle;
In a preferred embodiment, step b may further comprise the steps:
Open T-valve, pass into inert gas in the solution cylinder and discharge whole liquid in the solution cylinder, until be the inert gas space of anaerobic in the solution cylinder;
Will treat the reaction solution of deoxygenation inject in the solution cylinder, agitating solution, and in the solution cylinder inert gas injecting, when the pressure in the solution cylinder increases, to the pressure release of solution cylinder and exhaust;
The value of the dissolved oxygen DO in the control solution cylinder reaches when setting and stops to pass into inert gas, and the Pressure Drop in the solution cylinder to atmospheric pressure, is stopped stirring reaction solution, namely finishes the deoxygenation operation.
The invention has the beneficial effects as follows: can accurately control the oxygen content of solution, autoclave is controlled at anaerobic state, and under anaerobic state, incite somebody to action the reaction solution injection autoclave of deoxygenation, solve well the problem of accurate control solution oxygen content.
Description of drawings
Fig. 1 is the described structural representation of controlling the device of dissolved oxygen DO in reaction vessel of the embodiment of the invention;
Description of reference numerals:
1-solution cylinder, 2-top cover, 3-liquid phase sample valve, 4-gas phase sample valve, 5-autoclave kettle, 6-gas bomb, the 7-dissolved oxygen probe, 8-stirrer, 9-stirring vane, the 10-draft tube, 11-controller, 12-T-valve, the 13-pressure limiting valve, 14-safety valve, 15-liquid feed valve, the 16-vent valve, the 17-gas admittance valve.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated.
Embodiment:
As shown in Figure 1, a kind of device of controlling dissolved oxygen DO in reaction vessel comprises the solution cylinder 1 with top cover 2, the autoclave with liquid phase sample valve 3 and gas phase sample valve 4.Described gas phase sample valve 4 is connected to for the gas bomb 6 that stores inert gas, is provided with dissolved oxygen probe 7 in the described solution cylinder 1, by the stirring vane 9 of stirrer 8 controls be connected connecting the draft tube 10 of the gas bomb 6 of storage inert gas.Described dissolved oxygen probe 7 all connects into controller 11 with described stirrer 8, and the bottom of described solution cylinder 1 is connected with liquid phase sample valve 3 by T-valve 12.The outside surface of described top cover 2 is provided with pressure limiting valve 13, safety valve 14, liquid feed valve 15 and the vent valve 16 that communicates with solution cylinder 1 inside, and the top of described liquid feed valve 15 is higher than the top of described vent valve 16, and described draft tube 10 is provided with gas admittance valve 17.
In the present embodiment, described top cover 2 is sealedly attached to the top of described solution cylinder 1 by packing washer, and purpose is the impermeability that guarantees whole system.Described solution cylinder 1 is the graduated container of tool, and purpose is to limit the volume that imports solution.Described safety valve 14 is spring safety valve, and purpose is to guarantee that safety valve 14 can use well.Described gas admittance valve 17 is located at the top of described top cover 2, and purpose is to guarantee smoothly operation and adjust gas admittance valve 17.Described controller 11 is provided with display device, and purpose is the numerical value of being convenient to observe control.
In the present embodiment, the first connector of described T-valve 12 is connected in the bottom sides of described solution cylinder 1, and the second connector connects the conduit that described liquid phase sample valve 3, the joint among three members connections communicate with atmosphere.
In the present embodiment, pressure limiting valve 13 places top cover 2 outside surfaces to keep cylinder pressure constant; Gas admittance valve 17 places top cover 2 tops and connects up and down draft tube 10, and top cover 2 top draft tube 10 link to each other with source of the gas, and bottom draft tube 10 places in the solution cylinder 1, makes air inlet pass into the solution bottom; Dissolved oxygen probe 7 places top cover 2 bottoms, and dissolved oxygen probe 7 placed solution after top cover 2 was installed on the solution cylinder 1; Stirrer 8 is installed on the top cover 2, in order to guarantee the even of solution; Controller 11 is connected with dissolved oxygen probe 7 and stirrer 8, to show and to record the numerical value of dissolved oxygen DO and control stirring rate; Safety valve 14 guaranteed solution cylinder 1 internal pressure safety when pressure limiting valve 13 lost efficacy; Liquid feed valve 15 is in order to dosing in cylinder; Vent valve 16 places top cover 2, makes cylinder pressure identical with atmospheric pressure when it is opened.Pressure limiting valve 13 discharges gas to guarantee the constant pressure in the solution cylinder 1 in the excessive situation of the rear pressure of solution cylinder 1 sealing, prevent that simultaneously air from entering in the solution cylinder 1; Gas admittance valve 17 is used for controlling inert gas and enters in the solution cylinder 1; Dissolved oxygen probe 7 places solution to measure the solution oxygen content; Stirrer 8 in order to guarantee the homogeneity of solution, reaches the purpose of even deoxygenation when the ventilation deoxygenation; T-valve 12 usefulness derive the solution of deoxygenation, and can carry out sampling and the discharge opeing of an interior liquid; Controller 11 is used for showing and the record dissolved oxygen content observe whether oxygen content reaches requirement and adjust stirrer 8 rotational speeies in the solution; When safety valve 14 is used for pressure limiting valve 13 inefficacy, guarantee solution cylinder 1 safety; Liquid feed valve 15 is used for to solution cylinder 1 interior adding medicament; Vent valve 16 guarantees that when dosing solution cylinder 1 internal pressure equals atmospheric pressure, and is used for Exhaust Gas.
For the described device of above-described embodiment, the inventor has also designed a kind of method of controlling dissolved oxygen DO in reaction vessel, may further comprise the steps:
A. in autoclave, fill with water or other liquid, again the water in the autoclave or liquid are discharged with inert gas, make to be oxygen-free environment in the autoclave;
Step a may further comprise the steps:
In solution cylinder 1, be full of water or other liquid, pass into inert gas in the solution cylinder 1 again water or liquid are pressed out in the autoclave kettle 5;
After in autoclave kettle 5, filling with water or other liquid, stop in solution cylinder 1, passing into inert gas;
Open T-valve 12 autoclave kettle 5 is linked to each other with atmosphere, pass into inert gas in the autoclave kettle 5 water or other liquid in the autoclave kettle 5 are discharged, until be the inert gas space of anaerobic in the autoclave kettle 5;
B. will treat that the reaction solution of deoxygenation injects the solution cylinder 1 of anaerobic, and in solution cylinder 1, pass into inert gas and keep solution cylinder 1 interior positive pressure environment that reaction solution is carried out deoxygenation, and control it and reach setting value and namely finish deoxygenation;
Step b may further comprise the steps:
Open T-valve 12, pass into inert gas in the solution cylinder 1 and discharge whole liquid in the solution cylinder 1, until be the inert gas space of anaerobic in the solution cylinder 1;
The reaction solution for the treatment of deoxygenation is injected in the solution cylinder 1, agitating solution, and to solution cylinder 1 interior inert gas injecting, when the pressure in the solution cylinder 1 increases, to 1 pressure release of solution cylinder and exhaust;
The value of the dissolved oxygen DO in the control solution cylinder 1 reaches and stops to pass into inert gas when setting, and the Pressure Drop in the solution cylinder 1 to atmospheric pressure, is stopped stirring reaction solution, namely finishes the deoxygenation operation.
C. the reaction solution with deoxygenation passes in the autoclave under the environment that does not contact oxygen.
Next the inventor describes by concrete example:
The technology path that this example adopts is: reaction vessel is controlled at anaerobic state, and incites somebody to action the reaction solution injection reaction vessel of deoxygenation under anaerobic state.
The major function of this example is: dissolved oxygen content reaches experiment or research necessary requirement in the control reaction vessel solution, and other parameter of capable of regulating (such as pH, ion concentration) in use.The key technical indexes: dissolved oxygen content measurement range: 0 μ g/L-100.0 μ g/L, 0mg/L-20.0mg/L; Volume: 2L/5L.Service condition: supply voltage: 220V; Supply frequency 50Hz; Working temperature: 0-60 ℃.
Concrete control method is as follows:
1, cleans autoclave, keep cleaning in the autoclave;
2, use step that autoclave is sealed according to autoclave;
3, according to Fig. 1 gas admittance valve 17 is linked to each other with the gas cylinder that stores inert gas, check whether connection is tight, opens the gas cylinder switch;
4, one of T-valve 12 is linked to each other with the liquid phase sample valve 3 of autoclave;
5, open vent valve 16, from liquid feed valve 15 pure water is injected in the solution cylinder 1, discharge (liquid feed valve 15 ends are higher than vent valve 16) by vent valve 16 to pure water.Close liquid feed valve 15, close vent valve 16, fill with pure water in the solution cylinder 1 at this moment;
6, the liquid phase sample valve 3 of opening high pressure reactor and gas phase sample valve 4 are opened T-valve 12 the liquid phase sample valve 3 of autoclave are communicated with solution cylinder 1, open gas admittance valve 17 and pass into inert gas;
7, when pure water is flowed out by gas phase sample valve 4, close successively gas admittance valve 17, T-valve 12, fill with pure water in the autoclave kettle 5 at this moment;
8, gas phase sample valve 4 is linked to each other with the gas cylinder that stores inert gas, opening T-valve 12 makes autoclave kettle 5 link to each other with atmosphere, open gas cylinder, to the high pressure reactor liquid phase sample valve 3 during Exhaust Gas, close gas cylinder, close gas phase sample valve 4, close liquid phase sample valve 3, closing T-valve 12, is the inert gas space of anaerobic in the autoclave kettle 5 at this moment;
9, opening T-valve 12 solution cylinder 1 is linked to each other with atmosphere, open gas admittance valve 17, close gas admittance valve 17 behind discharge solution cylinder 1 interior whole liquid, close T-valve 12, is the inert gas space of anaerobic in the solution cylinder 1 at this moment;
10, open liquid feed valve 15 and vent valve 16, will treat that by liquid feed valve 15 deoxygenation solution injects solution cylinder 1, closes liquid feed valve 15 and vent valve 16;
11, open the power supply of controller 11, adjust the speed of stirrer 8, open gas admittance valve 17.When pressure increases, rely on 13 pairs of solution cylinders of pressure limiting valve 1 to carry out pressure release and exhaust;
12, observe controller 11, close gas admittance valve 17 to the dissolved oxygen DO displayed value during for the control required value, open fast and close vent valve 16 and make solution cylinder 1 Pressure Drop to atmospheric pressure, and after 5 minutes, observe the reading of controller 11;
If dissolved oxygen content does not reach requirement in 13 solution, then continue to open gas admittance valve 17, until dissolved oxygen content reaches requirement, and do not change in 5 minutes, gas admittance valve 17 is closed condition;
14, open gas admittance valve 17, to pressure limiting valve 13 Exhaust Gas, close gas admittance valve 17, close stirrer 8;
15, open successively liquid phase sample valve 3, gas phase sample valve 4, T-valve 12, solution cylinder 1 is linked to each other with autoclave kettle 5;
16, after being pressed into certain volume solution in the autoclave kettle 5, close successively T-valve 12, autoclave liquid phase sample valve 3, gas phase sample valve 4, closing controller 11 power supplys are removed the connection that liquid phase sample valve 3 is connected with T-valve, finish the deoxygenation operation.
More than in the operation, following points for attention are arranged:
(1) if solution condition changes or when adjusting to deoxygenation solution adding medicine after the deoxygenation, can open liquid feed valve 15 and vent valve 16 carries out feeding operations;
(2) should prevent that dissolved oxygen probe 7 surfaces from gas absorption occuring, and affects measurement result;
When (3) passing into the deoxygenation reaction solution of certain volume by T-valve 12 to autoclave, should close stirrer 8 and gas admittance valve 17, steady to guarantee liquid level;
(4) for whether change after the test solution deoxygenation (such as pH), can carry out sample analysis by T-valve 12 atmosphere one end;
(5) pass into pure water through GCF1 type permanent magnetism is rotated autoclave, and import N by gas phase sample valve 4 2After the pure water discharge, find that last solution is less in the kettle, can ignore to the change of autoclave kettle 5 required importing solution concentrations and oxygen content;
The horizontal positioned that (6) should keep reaction vessel to reach.
The above embodiment has only expressed the specific embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.

Claims (10)

  1. One kind in reaction vessel control dissolved oxygen DO device, comprise the solution cylinder with top cover, it is characterized in that, also comprise the autoclave with liquid phase sample valve and gas phase sample valve, described gas phase sample valve is connected to for the gas bomb that stores inert gas, be provided with dissolved oxygen probe in the described solution cylinder, stirring vane and the draft tube that is connected connecting the gas bomb that stores inert gas by stirrer control, described dissolved oxygen probe and described stirrer all connect into controller, the bottom of described solution cylinder is connected with the liquid phase sample valve by T-valve, the outside surface of described top cover is provided with the pressure limiting valve that communicates with solution cylinder inside, safety valve, liquid feed valve and vent valve, the top of described liquid feed valve is higher than the top of described vent valve, and described draft tube is provided with gas admittance valve.
  2. 2. the device of controlling dissolved oxygen DO in reaction vessel according to claim 1 is characterized in that described top cover is sealedly attached to the top of described solution cylinder by packing washer.
  3. 3. the device of controlling dissolved oxygen DO in reaction vessel according to claim 1 and 2 is characterized in that described solution cylinder is the graduated container of tool.
  4. 4. the device of controlling dissolved oxygen DO in reaction vessel according to claim 1 and 2 is characterized in that described safety valve is spring safety valve.
  5. 5. the device of controlling dissolved oxygen DO in reaction vessel according to claim 1 and 2 is characterized in that described gas admittance valve is located at the top of described top cover.
  6. 6. the device of controlling dissolved oxygen DO in reaction vessel according to claim 1 and 2 is characterized in that described controller is provided with display device.
  7. According to claim 1 and 2 in reaction vessel control dissolved oxygen DO device, it is characterized in that, the first connector of described T-valve is connected in the bottom sides of described solution cylinder, and the second connector connects described liquid phase sample valve, the conduit that the joint among three members connection communicates with atmosphere.
  8. 8. the method for a control dissolved oxygen DO in reaction vessel is characterized in that, may further comprise the steps:
    A. in autoclave, fill with water or other liquid, again the water in the autoclave or liquid are discharged with inert gas, make to be oxygen-free environment in the autoclave;
    B. will treat that the reaction solution of deoxygenation injects the solution cylinder of anaerobic, and pass into inert gas in the solution cylinder and keep in the solution cylinder positive pressure environment that reaction solution is carried out deoxygenation, and control it and reach setting value and namely finish deoxygenation;
    C. the reaction solution with deoxygenation passes in the autoclave under the environment that does not contact oxygen.
  9. According to claim 8 in reaction vessel control dissolved oxygen DO method, it is characterized in that step a may further comprise the steps:
    In the solution cylinder, be full of water or other liquid, pass into inert gas in the solution cylinder again water or liquid are pressed out in the autoclave kettle;
    After in the autoclave kettle, filling with water or other liquid, stop in the solution cylinder, passing into inert gas;
    Open T-valve the autoclave kettle is linked to each other with atmosphere, pass into inert gas in the autoclave kettle water or other liquid in the autoclave kettle are discharged, until be the inert gas space of anaerobic in the autoclave kettle.
  10. According to claim 8 in reaction vessel control dissolved oxygen DO method, it is characterized in that step b may further comprise the steps:
    Open T-valve, pass into inert gas in the solution cylinder and discharge whole liquid in the solution cylinder, until be the inert gas space of anaerobic in the solution cylinder;
    Will treat the reaction solution of deoxygenation inject in the solution cylinder, agitating solution, and in the solution cylinder inert gas injecting, when the pressure in the solution cylinder increases, to the pressure release of solution cylinder and exhaust;
    The value of the dissolved oxygen DO in the control solution cylinder reaches when setting and stops to pass into inert gas, and the Pressure Drop in the solution cylinder to atmospheric pressure, is stopped stirring reaction solution, namely finishes the deoxygenation operation.
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Cited By (5)

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CN103326049A (en) * 2013-06-19 2013-09-25 大连融科储能技术发展有限公司 Hydrogen discharging system of redox flow battery
CN105833750A (en) * 2016-03-18 2016-08-10 上海化工研究院 Sealing type gas quantitative dissolving device and application thereof
CN106371470A (en) * 2016-08-24 2017-02-01 安科工程技术研究院(北京)有限公司 Corrosion evaluation test dissolved oxygen content control device and method
CN106557094A (en) * 2016-11-30 2017-04-05 清华大学 Dissolved oxygen content precise control device in a kind of liquid fuel
CN106698308A (en) * 2017-01-23 2017-05-24 山东新贵科技股份有限公司 Method for controlling oxygen solubility of original beer in cold-chain logistics process

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