CN111111481A - Manufacturing system and method for trace dissolved ternary mixed gas standard solution - Google Patents
Manufacturing system and method for trace dissolved ternary mixed gas standard solution Download PDFInfo
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- CN111111481A CN111111481A CN202010061632.4A CN202010061632A CN111111481A CN 111111481 A CN111111481 A CN 111111481A CN 202010061632 A CN202010061632 A CN 202010061632A CN 111111481 A CN111111481 A CN 111111481A
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- 239000012086 standard solution Substances 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims description 31
- 239000007789 gas Substances 0.000 claims abstract description 208
- 239000007788 liquid Substances 0.000 claims abstract description 72
- 239000012159 carrier gas Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000011550 stock solution Substances 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000005507 spraying Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 230000007246 mechanism Effects 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000009795 derivation Methods 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000009423 ventilation Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 230000002457 bidirectional effect Effects 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 7
- 238000007789 sealing Methods 0.000 description 7
- 230000005855 radiation Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 230000001174 ascending effect Effects 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003113 dilution method Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
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- 230000008569 process Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/10—Mixing gases with gases
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/20—Mixing gases with liquids
- B01F23/23—Mixing gases with liquids by introducing gases into liquid media, e.g. for producing aerated liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/45—Magnetic mixers; Mixers with magnetically driven stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
- B01F33/821—Combinations of dissimilar mixers with consecutive receptacles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/93—Heating or cooling systems arranged inside the receptacle
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/99—Heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/211—Measuring of the operational parameters
- B01F35/2111—Flow rate
- B01F35/21111—Mass flow rate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/211—Measuring of the operational parameters
- B01F35/2113—Pressure
Abstract
The embodiment of the invention discloses a manufacturing system of a trace dissolved ternary mixed gas standard solution, which comprises a fixed proportion gas conveying unit; the gas mixing unit is used for mixing the component gas and the carrier gas supplied by the fixed-proportion gas conveying unit to obtain intermediate gas; a liquid supply unit for supplying high-purity cleaning water and spraying stock solution; and calibrating the volume and the gas pressure of the intermediate gas in a constant-temperature sealed environment to obtain target gas, calibrating the volume of stock solution in a constant-temperature sealed environment to obtain target liquid, continuously stirring and mixing the target gas and the target liquid to obtain standard solution, discharging the standard solution dynamically out of a liquid mixer, controlling the mass flow of the gas by a high-precision mass flow controller, fully mixing the gas and the solution in a multiple mixing mode, and finally outputting the dynamic standard solution which is not influenced by the temperature and pressure condition and does not generate any waste gas or waste liquid harmful to the environment.
Description
Technical Field
The embodiment of the invention relates to the technical field of preparation of trace dissolved ternary mixed gas standard solutions, and particularly relates to a manufacturing system and method of a trace dissolved ternary mixed gas standard solution.
Background
The standard mixed gas is prepared by taking a high-purity gas as a diluent gas and adding one or more other high-purity gases, and mainly comprises a weighing method, a partial pressure method, a volume method, a permeation method, a saturation method, an electrolysis method, an index dilution method and the like. The preparation of the standard solution mostly adopts methods such as a volumetric method, a neutralization method, a redox method, a complex titration method, a method for manufacturing a system for preparing the quantitative trace water-soluble gas standard solution and the like.
Wherein, standard gas preparation methods such as a weighing method, a partial pressure method, a volume method, a permeation method, a saturation method, an electrolysis method, an index dilution method and the like are only suitable for preparing constant value mixed standard gas;
the preparation methods of standard solutions such as a volumetric method, a neutralization method, a redox method, a complex titration method and the like are only suitable for preparing the standard solution taking non-gas as a main target;
the method for manufacturing the constant value trace water-soluble gas standard solution can manufacture the standard solution taking water-soluble gas as a main target according to a headspace balance gas chromatography testing principle, but can be realized by depending on a plurality of systems such as a pressure-resistant stock solution barrel, a constant gas standard solution preparation device, a gas chromatography unit and the like, and belongs to a static manufacturing method from the aspect of dynamics, the quantity of the standard solution manufactured each time is limited, and continuous output cannot be provided;
the existing methods can not meet the requirement of dynamic manufacturing of the standard solution of trace dissolved ternary mixed gas.
Disclosure of Invention
Therefore, the embodiment of the invention provides a system and a method for manufacturing a trace dissolved ternary mixed gas standard solution, which solve the problem that the conventional method cannot meet the dynamic manufacturing requirement of the trace dissolved ternary mixed gas standard solution.
In order to achieve the above object, an embodiment of the present invention provides the following:
a system for preparing a trace dissolved ternary mixed gas standard solution comprises
The fixed proportion gas conveying unit is used for providing component gas and carrier gas in preset proportion;
the gas mixing unit is used for mixing the component gas and the carrier gas supplied by the fixed-proportion gas conveying unit to obtain intermediate gas;
the liquid supply unit is used for providing high-purity cleaning water and spraying stock solution;
and the gas-liquid mixer is used for calibrating the volume and the gas pressure of the intermediate gas in a constant-temperature sealed environment to obtain target gas, calibrating the volume of stock solution in a constant-temperature sealed environment to obtain target liquid, continuously stirring and mixing the target gas and the target liquid to obtain standard solution, and dynamically discharging the standard solution.
As a preferable mode of the present invention, the fixed-ratio delivery unit includes a plurality of first branch pipes for component gas delivery and a second branch pipe for carrier gas delivery, and a vacuum system that realizes a near vacuum state of the first branch pipes, the second branch pipes, the gas mixing unit, and the gas-liquid mixer.
As a preferable aspect of the present invention, a pressure sensor and a mass flow controller are mounted on the first branch pipe, the second branch pipe, and the pipe of the vacuum system.
As a preferable scheme of the present invention, the gas mixing unit includes a main branch pipeline connecting the vacuum system and the gas-liquid mixer, and a turbofan gas mixing mechanism disposed on the main branch pipeline, the turbofan gas mixing mechanism is connected to the proportional gas delivery unit and receives the component gas and the carrier gas, and a ventilation coil pipe for spraying a mixed gas of the component gas and the carrier gas is disposed at a terminal of the main branch pipeline extending into the gas-liquid mixer;
the main branch pipeline positioned in the gas-liquid mixer is provided with a spiral pipe, and the main branch pipeline positioned between the spiral pipe and the turbofan gas mixing mechanism is connected through a quick joint.
As a preferable aspect of the present invention, the turbofan gas mixing mechanism is connected to a straight pipe main body of the target gas, which is mixed by a gas-liquid mixer and discharged through a relief valve provided in the gas-liquid mixer, and the straight pipe main body is provided with a check valve.
As a preferable aspect of the present invention, an internal pressure sensor for monitoring a top air pressure in the gas-liquid mixer is provided inside the pressure release valve, and an electrical signal of the top air pressure in the gas-liquid mixer acquired by the internal pressure sensor is used as a driving signal for operating the check valve.
As a preferred scheme of the invention, the gas-liquid mixer specifically comprises a mixing bin body, the gas proportional conveying mechanism is connected with the mixing bin body through a main branch pipeline, a stirring mechanism used for forming convection with gas sprayed by a vent coil is arranged in the mixing bin body, a magnetic heating stirrer is arranged at the bottom of the mixing bin body, and a stirrer driven to rotate by the magnetic heating stirring mechanism is arranged at the bottom in the mixing bin body;
the liquid supply unit comprises a water inlet pipe, a stock solution inlet pipe and a marking solution outlet pipe which are arranged on the mixing bin body, and the tail end of the stock solution inlet pipe, which is positioned in the mixing bin body, is connected with a water spraying coil pipe.
As a preferable scheme of the invention, a heat-preservation water jacket is arranged in the inner wall of the mixing bin body, and a medium in the heat-preservation water jacket is heated by a magnetic heating and stirring mechanism.
The invention provides a method for preparing a trace dissolved ternary mixed gas standard solution, which comprises the following specific steps:
s100, preliminarily mixing the component gas and the carrier gas according to a preset proportion to obtain intermediate gas;
s200, continuously introducing the intermediate gas into a constant-temperature closed environment, and simultaneously heating and stirring for secondary mixing;
s300, when the air pressure in the constant-temperature closed environment reaches a preset pressure value, obtaining target gas, stopping introducing intermediate gas, and simultaneously adding stock solution into the constant-temperature closed environment until the target gas is completely discharged out of the constant-temperature closed environment;
s400, after the liquid pressure in the sealed environment to be heated is stable, continuously introducing intermediate gas in the state of continuous stirring of the magnetic stirrer, keeping the stock solution continuously introduced to obtain a standard solution, and continuously and dynamically outputting the standard solution.
As a preferable scheme of the present invention, the preset proportion of the component gas and the carrier gas is based on obtaining a dilution ratio of the component gas and the carrier gas by the component gas initial concentration, the component gas flow rate, the carrier gas flow rate, the mixed gas outlet flow rate of the component gas and the carrier gas, and the dynamic output target liquid flow rate, and further obtaining a ratio of the flow rate of each component gas and the carrier gas flow rate by derivation calculation.
The embodiment of the invention has the following advantages:
the high-precision mass flow controller controls the mass flow of gas, and fully and uniformly mixes the gas and the solution through multiple mixing modes such as a spiral pipe, a ventilating coil pipe, a three-dimensional spiral mixing blade, a magnetic heating stirrer and the like, and finally outputs the dynamic standard solution.
The preparation process of the standard solution is not influenced by temperature and pressure conditions, does not generate any waste gas or waste liquid harmful to the environment, has high preparation efficiency, high precision, sustainable dynamic output, safety, stability, greenness, environmental protection, simple device, low cost and simple and convenient operation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions that the present invention can be implemented, so that the present invention has no technical significance, and any structural modifications, changes in the ratio relationship, or adjustments of the sizes, without affecting the effects and the achievable by the present invention, should still fall within the range that the technical contents disclosed in the present invention can cover.
FIG. 1 is a block diagram of a system for producing a trace dissolved ternary mixed gas standard solution according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a fixed-ratio gas delivery mechanism according to an embodiment of the present invention;
FIG. 3 is a schematic view of a blade configuration according to an embodiment of the present invention;
FIG. 4 is a schematic flow chart illustrating a method for controlling the production of a standard mixed gas solution according to an embodiment of the present invention;
FIG. 5 is a schematic view of a quick connector structure according to an embodiment of the present invention;
FIG. 6 is a schematic view of a gas-liquid mixer in an embodiment of the present invention;
FIG. 7 is a block diagram of a manufacturing system in accordance with an embodiment of the present invention.
In the figure:
1-a first branch pipe; 2-a second branch pipe; 3-a vacuum system; 4-a pressure sensor; 5-a mass flow controller; 6-total branch pipeline; 7-turbofan gas mixing mechanism; 8-aeration coil pipe; 9-a spiral pipe; 10-a quick coupling; 11-a straight tube body; 12-an internal pressure sensor; 13-a wire mesh separator; 14-a pressure relief valve; 15-a one-way valve; 16-a mixing bin body; 17-a water inlet pipe; 18-raw liquid inlet pipe; 19-a marker liquid outlet pipe; 20-water spraying coil pipe; 21-a central rotating shaft; 22-magnetic heating stirring mechanism; 23-a stirrer; 24-heat preservation water jacket; 25-a stationary ring; 26-a blade; 27-inner blade; 28-outer blades; 29-flow deflectors; 30-a radiation rod;
101-a bidirectional pipe body; 102-a threaded segment; 103-threaded sleeve; 104-reducing layer sleeve; 105-an equal diameter tube; 106-projection; 107-annular groove; 108-embedded ring grooves; 109-annular latch tongue; 110-inner seal ring;
701-an upper chamber; 702-a lower chamber; 703-turbofan.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in FIG. 7, the present invention provides a system for preparing a trace dissolved ternary mixed gas standard solution, comprising
The fixed proportion gas conveying unit is used for providing component gas and carrier gas in preset proportion;
the gas mixing unit is used for mixing the component gas and the carrier gas supplied by the fixed-proportion gas conveying unit to obtain intermediate gas;
the liquid supply unit is used for providing high-purity cleaning water and spraying stock solution;
and the gas-liquid mixer is used for calibrating the volume and the gas pressure of the intermediate gas in a constant-temperature sealed environment to obtain target gas, calibrating the volume of stock solution in a constant-temperature sealed environment to obtain target liquid, continuously stirring and mixing the target gas and the target liquid to obtain standard solution, and dynamically discharging the standard solution.
As shown in fig. 1 to 6, the present invention provides a gas control system for the above component gas and carrier gas, comprising a proportional gas delivery unit and a gas mixing unit, comprising a plurality of first branch pipes 1 for component gas delivery and a second branch pipe 2 for carrier gas delivery, and a vacuum system 3 for realizing near vacuum state of the first branch pipe 1, the second branch pipe 2|, the gas mixing unit and the mixer.
The pipelines of the first branch pipe 1 and the second branch pipe 2 and the vacuum system 3 are respectively provided with a pressure sensor 4 and a mass flow controller 5, the pressure, the flow and the mass of the gas in the conveying pipeline are detected in real time, the flow and the mass in the conveying pipeline are adjusted in real time through the mass flow controller 5,
the present invention also provides a straight-through valve at both ends of the first branch pipe 1 and the second branch pipe at the mass flow controller 5, which functions to close the conveying state in the conveying pipeline and to start the vacuum system 3 by closing the straight-through valve, facilitating the completion of the near vacuum state in the conveying pipeline.
The component gas supply means of the first branch pipe 1 may be a gas supply cylinder and the carrier gas supply means of the second branch pipe 2 may be a gas carrier cylinder.
The invention further provides a preliminary mixing device for mixing the carrier gas and the component gas, namely a gas mixing unit, which specifically comprises the gas mixing unit, wherein the gas mixing unit comprises a main branch pipeline 6 connected with a vacuum system 3 and a mixer and a turbofan 703 gas mixing mechanism 7 arranged on the main branch pipeline 6, the turbofan 703 gas mixing mechanism 7 is connected with a proportional gas conveying unit and receives the component gas and the carrier gas, and the tail end of the main branch pipeline 6 extending into the mixer is provided with a ventilation coil 8 for spraying the mixed gas of the component gas and the carrier gas;
the mixed gas flow delivered by the fixed-proportion gas delivery unit is changed by the turbofan 703 gas mixing mechanism 7, and the flow rate of the mixed gas delivered to the mixer from the main branch pipeline 6 is controlled by the turbofan 703 gas mixing mechanism 7.
The main branch pipe positioned in the mixed gas is provided with a spiral pipe 9, and the main branch pipe positioned between the spiral pipe 9 and the turbofan 703 gas mixing mechanism 7 is connected through a quick joint 10.
The turbofan 703 gas mixing mechanism 7 comprises an upper chamber 701 for connecting the first branch pipe 1 and a lower chamber 702 for connecting the second branch pipe 2 and for mixing the carrier gas and the component gas, wherein the upper chamber 701 and the lower chamber 702 are internally provided with a turbofan 703 coaxially rotating, and the interiors of the upper chamber 701 and the lower chamber 702 are in a communicated state;
further, the turbofan 703 in the upper chamber 701 and the lower chamber 702 may rotate coaxially or may rotate by two rotating shafts, respectively.
The vacuum system 3 is connected by piping to the connection of the second branch pipe 2 to the lower chamber 702.
During operation, the component gas flows into the turbofan 703 gas mixing mechanism 7 through the first branch pipe 1, is mixed with the carrier gas entering the lower chamber 702 through the second branch pipe 2 after being primarily mixed in the upper chamber 701, and finally is sent to the spiral pipe 9 through the main branch pipe, and finally is sprayed out through the ventilating coil pipe 8.
The straight pipe main body 11 of the target gas mixed by the gas-liquid mixer and discharged through a relief valve 14 provided in the gas-liquid mixer is connected to the lower chamber 702.
The straight pipe body 11 is provided therein with a wire mesh separator 13 for gas-liquid separation, and the straight pipe body 11 is provided with a check valve 15.
The pressure relief valve 14 is provided with an internal pressure sensor 12 for monitoring the top gas pressure in the gas-liquid mixer, and an electric signal of the top gas pressure in the gas-liquid mixer acquired by the internal pressure sensor 12 is used as a driving signal for the operation of the check valve 15.
When the air pressure of target gas in a gas-liquid mixer in a constant-temperature closed environment reaches a preset pressure value, stopping introducing intermediate gas, and simultaneously adding a pre-prepared stock solution into the constant-temperature gas-liquid mixer until the target gas is completely discharged out of the gas-liquid mixer;
after the liquid pressure in the gas-liquid mixer is stabilized, the stock solution is kept continuously introduced to obtain the standard solution, the standard solution is continuously and dynamically output, and when the standard solution is continuously output, the gas which is not completely dissolved with the stock solution overflows the surface of the stock solution under the influence of the flow of a standard solution outlet pipe which dynamically outputs the standard solution, and then is accumulated at the inner top of the gas-liquid mixer, when the pressure value of the target gas at the inner top of the gas-liquid mixer reaches the set value of a pressure release valve 14, an internal pressure sensor 12 transmits an electric signal, a check valve 15 on a straight pipe main body 11 is opened, so that the target gas at the inner top of the gas-liquid mixer enters a lower-layer chamber 702, and the target gas is circularly dissolved again.
Meanwhile, in order to not affect the standard solution entering the lower chamber 702 and further affect the proportion of the component gas and the carrier gas of the fixed proportion gas conveying mechanism, a wire mesh separator 13 for gas-liquid separation is arranged in the straight pipe main body 11, and the condition that the mixed gas of the component gas and the carrier gas in the lower chamber 702 reversely enters a gas-liquid mixer through a one-way valve 15 and further affects the calibration of the standard solution is avoided.
The invention further provides a gas-liquid mixing device for mixing the gas and the stock solution after the carrier gas and the component gas are mixed, namely a gas-liquid mixer, which specifically comprises a mixing bin body 16, wherein a gas proportion conveying mechanism is connected with the mixing bin body 16 through a general branch pipeline 6, the mixing bin body 15 is provided with a stirring mechanism which is used for forming convection with the gas sprayed out by the ventilating coil pipe 9 in the mixing bin body 16, the bottom of the mixing bin body 16 is provided with a magnetic heating stirrer 22, and the bottom in the mixing bin body 16 is provided with a stirrer 23 which is driven to rotate by the magnetic heating stirring mechanism 22;
the liquid supply unit comprises a water inlet pipe 17, a stock solution inlet pipe 18 and a marking solution outlet pipe 19 which are arranged on the mixing bin body 16, and the tail end of the stock solution inlet pipe 18 positioned inside the mixing bin body 16 is connected with a water spraying coil pipe 20.
The stirring mechanism comprises a central rotating shaft 21 and mixing blades which are arranged on the central rotating shaft 21 at equal intervals, each mixing blade comprises a fixed ring 25 which is in contact with the inner wall of the mixing cabin 16, and blades 26 which are spirally arrayed between the central rotating shaft 21 and the fixed ring 25, each blade 26 comprises an inner blade 27 which is used for forming descending flow and an outer blade 28 which is used for forming ascending flow and has a radial distance smaller than that of the inner blade 27, and a flow deflector 29 which is used for maintaining the flow direction of the ascending flow or the descending flow is arranged between the outer blade 28 and the inner blade 27.
The inner paddle 27 and the outer paddle 28 are connected to the same radiation rod 30 along the radial direction of the fixing ring, two ends of the radiation rod 30 are connected to the central rotating shaft 21 and the fixing ring 25 respectively, and the spiral directions of the inner paddle 27 and the outer paddle 28 are opposite.
The invention has two working states that are provided,
firstly, the central rotating shaft 21 can be driven to rotate by an external driving mechanism, such as an electric motor or a motor;
secondly, the air pipe 8 sprays directional gas into the mixing cabin 16 to form directional vortex flow for the liquid in the mixing cabin, or sprays directional water flow into the mixing cabin 16 through the water inlet pipe to form directional vortex flow, at this moment, the central rotating shaft 1 is fixedly installed on the mixing cabin 16, and the blades 3 are installed on the central rotating shaft through bearings.
And each blade of the paddle is provided with a strip-shaped through groove for guiding the water body.
The blades in any working state can realize that the water flow in the mixing bin body 16 forms a circulating water flow in the form of a magnetic field, for example, and the specific forming mode of the circulating water flow is as follows:
the water forms the rivers post under the rotation direction of paddle including and is just contacting with the air feed pipe who is located mixing storehouse body 16 bottom, because air feed pipe spun gas has certain play speed, and then can increase contact surface between them as far as, and under the water conservancy diversion effect of water conservancy diversion piece, the water circulation that forms interior paddle and outer paddle is separated, and the water circulation that forms interior paddle and outer paddle is from up circulating down, the contact route of gas and liquid has been increased, can make the gas-liquid intensive mixing.
The inner paddle and the outer paddle are connected to the same radiation rod along the radial direction of the fixing ring, two ends of the radiation rod are connected to the central rotating shaft and the fixing ring respectively, and the spiral directions of the inner paddle and the outer paddle are opposite.
Interior paddle and outer paddle have 2 ~ 3 cm's difference in height in the axial, and interior paddle and outer paddle reduce along the radial width of retainer plate gradually, there is the angle difference of 10 ~ 30 between interior paddle and the outer paddle, the velocity of flow of inside and outside rivers is different, interior paddle is because the paddle width will be greater than the width of outer paddle, just also make the rivers circulating speed that interior paddle formed slow with the velocity of flow that outer paddle formed, then make the velocity of flow that interior paddle formed and ventilating coil's spun gas contact time long.
Further, the ventilating coil 8 is specifically an annular pipe with uniformly distributed air holes.
The guide vane 29 is located between two adjacent inner blades 27, and two ends of the guide vane 29 are respectively connected to two adjacent radiation rods.
The tail end of the outer paddle is not completely connected with the inner wall of the fixing ring, and the cross section of the fixing ring is in the shape of an inverted normal distribution curve.
Furthermore, the invention also provides a stirring paddle utilizing the mixing blades, which comprises the steps that the mixing blades are arranged on a central rotating shaft at equal intervals, and the bottom of the central rotating shaft is provided with a plurality of supporting frames embedded on the bottom wall of the mixing bin body 16.
The ventilating coil 8 is positioned at the upper part of the stirrer 23 and sprays mixed gas upwards from the bottom of the mixing cabin 16, and the stock solution inlet pipe 18 is positioned on the side wall of the top of the mixing cabin 16.
Be provided with heat preservation water jacket 24 in the mixing storehouse body 16 inner wall, and the medium in the heat preservation water jacket 24 heats through magnetic force heating rabbling mechanism 22, and the stirring of the interior stirring of the mixed storehouse body 16 of magnetic force heating agitator drive 23 motion plays the stirring effect to gas to provide a homothermal mixed environment for mixing the storehouse body 16 in through heat preservation water jacket 24.
Further, the invention provides a quick coupling, which specifically comprises a bidirectional pipe body 101 and two threaded sleeves 103 which are spirally connected to the bidirectional pipe body 101 through a threaded section 102; wherein the threaded sleeve 103 is movably sleeved on the bidirectional pipe body 101, a hose for connecting a container tank in the process of manufacturing the constant value ternary mixed standard gas is sleeved at two ends of the bidirectional pipe body 101, the threaded sleeve 103 is rotated, so that the hose is sleeved between the threaded sleeve 103 and the bidirectional pipe body 101, the hose is pressed through the threaded sleeve 103, and the hose is unlocked by reversely rotating the threaded sleeve 103.
The joint department of traditional quick-operation joint 10 all is the direct anti-skidding arch 106 that sets up the layer cover, the direct suit of hose is on anti-skidding arch 106, carry out the high-speed joint of pipeline, and this kind of side of connection is unable to be suitable for under the especially higher condition of gaseous or liquid precision requirement in the laboratory, when intraductal atmospheric pressure or hydraulic pressure are the change, the junction of hose and quick-operation joint 10 produces inflation or shrink easily, and then make gaseous leakage or inhale the outside air, and then influence the result of experiment.
In the invention, the two ends of the bidirectional pipe body 101 are provided with the reducing layer sleeves 104, the tail ends of the reducing layer sleeves 104 are provided with the equal-diameter pipes 105, the equal-diameter pipes 105 are used for increasing the surfaces which are in parallel contact with the inner wall of the hose, and when the hose is sleeved with the equal-diameter pipes 105, no matter how the air pressure in the hose changes, the hose cannot expand and leak at the connecting part.
The constant diameter pipe 105 is provided with an annular groove 107 matched with a bulge 106 arranged inside the threaded sleeve 103, the joint of the reducing layer sleeve 104 and the bidirectional pipe body 101 is provided with a self-sealing structure, the self-sealing structure comprises an embedded ring groove 108 arranged on the bidirectional pipe body 101 and an annular pin tongue 109 arranged inside the threaded sleeve 103, and an inner sealing ring 110 is arranged in the embedded ring groove 108.
The invention also forms a sealing space to form a sealing chamber with stable pressure when the main branch pipeline 6 is sleeved with the reducing layer sleeve 104 by combining the threaded sleeve 103 and the reducing layer sleeve 104, can ensure the connection stability of the main branch pipeline 6 when the pressure in the hose is overlarge or overlook, and can not generate the air leakage condition.
An outer sealing ring is arranged on the bidirectional pipe body 101 positioned on the outer side of the embedded ring groove 108, the contact surface of the embedded ring groove 108 and the annular pin tongue 109 is an inclined surface, the inclination angle of the inclined surface is 10-20 degrees, and the axial length of the annular pin tongue 109 is 1-2 mm shorter than that of the embedded ring groove 108.
The threaded sleeve 103 comprises a straight pipe section and a circular truncated cone section inside, and the circular truncated cone section axially extends to the root of the annular pin tongue 109.
The diameter of each layer of the reducing layer sleeve 104 is gradually increased until the diameter is the same as that of the equal diameter pipe 105.
The bulge 106 comprises two adjacent semicircular bulge rings, a certain gap exists between the two bulge rings, the height of the bulge ring positioned on the inner side is higher than that of the bulge ring positioned on the outer side, the function of the bulge ring is that in the long-time sleeving process, a hose is clamped in the annular groove 107, the bulge ring on the outer side buckles the hose into the annular groove 107, and the deformed part of the hose is pressed and held on the surface of the equal-diameter pipe 105 by the bulge ring on the inner side, so that sealing is realized;
and be applicable to the hose that the pipe diameter has 2 ~ 3mm disparity, when cup jointing, the pipe diameter is thinner then with inboard protruding circle with the pipe wall of hose impressed annular groove 107, outside protruding circle with the hose lie in the annular groove 107 outside the part pressure hold on the equal diameter pipe 105 surface.
The invention provides a method for preparing a trace dissolved ternary mixed gas standard solution, which comprises the following specific steps:
s100, preliminarily mixing the component gas and the carrier gas according to a preset proportion to obtain intermediate gas;
s200, continuously introducing the intermediate gas into a constant-temperature closed environment, and simultaneously heating and stirring for secondary mixing;
s300, when the air pressure in the constant-temperature closed environment reaches a preset pressure value, obtaining target gas, stopping introducing intermediate gas, and simultaneously adding stock solution into the constant-temperature closed environment until the target gas is completely discharged out of the constant-temperature closed environment;
s400, after the liquid pressure in the sealed environment to be heated is stable, continuously introducing intermediate gas in the state of continuous stirring of the magnetic stirrer, keeping the stock solution continuously introduced to obtain a standard solution, and continuously and dynamically outputting the standard solution.
The preset proportion of the component gas and the carrier gas is based on the initial concentration of the component gas, the flow of the carrier gas, the outlet flow of the mixed gas of the component gas and the carrier gas and the dynamic output target liquid flow, the dilution ratio of the component gas and the carrier gas is obtained, and the ratio of the flow of each component gas to the flow of the carrier gas is obtained through derivation calculation.
In S300, the raw liquid is added to the closed environment at a constant temperature until the target gas is completely discharged from the closed environment at the constant temperature, and the pressure value of the target gas discharged from the closed environment at the constant temperature is set to 1 atm.
In S400, after the liquid pressure in the sealed environment to be heated is stable, the stable state of the liquid pressure is kept for 5 min.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A manufacturing system of a trace dissolved ternary mixed gas standard solution is characterized by comprising
The fixed proportion gas conveying unit is used for providing component gas and carrier gas in preset proportion;
the gas mixing unit is used for mixing the component gas and the carrier gas supplied by the fixed-proportion gas conveying unit to obtain intermediate gas;
the liquid supply unit is used for providing high-purity cleaning water and spraying stock solution;
and the gas-liquid mixer is used for calibrating the volume and the gas pressure of the intermediate gas in a constant-temperature sealed environment to obtain target gas, calibrating the volume of stock solution in a constant-temperature sealed environment to obtain target liquid, continuously stirring and mixing the target gas and the target liquid to obtain standard solution, and dynamically discharging the standard solution.
2. The system for manufacturing a trace dissolved ternary mixed gas standard solution according to claim 1, wherein the fixed-proportion delivery unit comprises a plurality of first branch pipes (1) for component gas delivery and a second branch pipe (2) for carrier gas delivery, and a vacuum system (3) for realizing the near vacuum state of the first branch pipe (1), the second branch pipe (2), the gas mixing unit and the gas-liquid mixer.
3. The system for manufacturing the trace dissolved ternary mixed gas standard solution according to claim 2, wherein the pipelines of the first branch pipe (1), the second branch pipe (2) and the vacuum system (3) are all provided with a pressure sensor (4) and a mass flow controller (5).
4. The system for manufacturing the trace dissolved ternary mixed gas standard solution according to claim 1, wherein the gas mixing unit comprises a main branch pipeline (6) for connecting the vacuum system (3) and the gas-liquid mixer, and a turbofan gas mixing mechanism (7) arranged on the main branch pipeline (6), the turbofan gas mixing mechanism (7) is connected with the proportional gas delivery unit and receives the component gas and the carrier gas, and the end of the main branch pipeline (6) extending into the gas-liquid mixer is provided with a vent coil (8) for ejecting mixed gas of the component gas and the carrier gas;
the main branch pipeline (6) positioned in the gas-liquid mixer is provided with a spiral pipe (9), and the main branch pipeline (6) positioned between the spiral pipe (9) and the turbofan gas mixing mechanism (7) is connected through a quick joint (10).
5. The system and the method for manufacturing the trace dissolved ternary mixed gas standard solution according to claim 4, wherein the turbofan gas mixing mechanism (7) is connected with a straight pipe main body (11) of the target gas which is mixed by a gas-liquid mixer and discharged through a pressure relief valve (14) arranged on the gas-liquid mixer, and a check valve (15) is arranged on the straight pipe main body (11).
6. The system for manufacturing the trace dissolved ternary mixed gas standard solution according to claim 5, wherein an internal pressure sensor (12) for monitoring the top gas pressure in the gas-liquid mixer is arranged inside the pressure release valve (14), and an electric signal of the top gas pressure in the gas-liquid mixer acquired by the internal pressure sensor (12) is used as a driving signal for the operation of the check valve (15).
7. The system for manufacturing the trace dissolved ternary mixed gas standard solution according to claim 1, wherein the gas-liquid mixer specifically comprises a mixing bin body (16), the gas proportional conveying mechanism is connected with the mixing bin body (16) through a general distribution pipeline (6), the mixing bin body (15) is provided with a stirring mechanism for forming convection with gas sprayed by a ventilation coil (8) inside the mixing bin body (16), a magnetic heating stirrer (22) is arranged at the bottom of the mixing bin body (16), and a stirrer (23) driven to rotate by the magnetic heating stirrer (22) is arranged at the bottom inside the mixing bin body (16);
the liquid supply unit comprises a water inlet pipe (17), a stock solution inlet pipe (18) and a marking solution outlet pipe (19) which are arranged on the mixing bin body (16), and the tail end of the stock solution inlet pipe (18) which is positioned inside the mixing bin body (16) is connected with a water spraying coil pipe (20).
8. The system for manufacturing the trace dissolved ternary mixed gas standard solution according to claim 7, wherein a heat-preservation water jacket (24) is arranged in the inner wall of the mixing bin body (16), and a medium in the heat-preservation water jacket (24) is heated by a magnetic heating stirring mechanism (22).
9. A manufacturing method of a trace dissolved ternary mixed gas standard solution is characterized by comprising the following specific steps:
s100, preliminarily mixing the component gas and the carrier gas according to a preset proportion to obtain intermediate gas;
s200, continuously introducing the intermediate gas into a constant-temperature closed environment, and simultaneously heating and stirring for secondary mixing;
s300, when the air pressure in the constant-temperature closed environment reaches a preset pressure value, obtaining target gas, stopping introducing intermediate gas, and simultaneously adding stock solution into the constant-temperature closed environment until the target gas is completely discharged out of the constant-temperature closed environment;
s400, after the liquid pressure in the sealed environment to be heated is stable, continuously introducing intermediate gas in the state of continuous stirring of the magnetic stirrer, keeping the stock solution continuously introduced to obtain a standard solution, and continuously and dynamically outputting the standard solution.
10. The method for preparing a trace dissolved ternary mixed gas standard solution according to claim 9, wherein the preset proportion of the component gas and the carrier gas is based on the component gas initial concentration, the component gas flow rate, the carrier gas flow rate, the mixed gas outlet flow rate of the component gas and the carrier gas, and the dynamic output target liquid flow rate, so as to obtain the dilution ratio of the component gas and the carrier gas, and further obtain the ratio of the flow rate of each component gas and the carrier gas flow rate through derivation calculation.
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| CN116272588A (en) * | 2023-04-17 | 2023-06-23 | 防灾科技学院 | Automatic manufacturing system for trace dissolved ternary mixed gas standard solution |
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