CN106370692B - The solution modeling visual inspection device of trace soluble impurity in cryogenic liquid - Google Patents
The solution modeling visual inspection device of trace soluble impurity in cryogenic liquid Download PDFInfo
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- CN106370692B CN106370692B CN201610743290.8A CN201610743290A CN106370692B CN 106370692 B CN106370692 B CN 106370692B CN 201610743290 A CN201610743290 A CN 201610743290A CN 106370692 B CN106370692 B CN 106370692B
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Abstract
The invention discloses a kind of solution modeling visual inspection devices of trace soluble impurity in cryogenic liquid, including integrated glass test unit, high speed microimaging unit, deep cooling solvent filling unit, soluble impurity filling unit, cooling medium to survey control temperature unit, vacuum unit and vaporizing, discharging pipe-line cell.The integrated glass test unit almost protects collet all standing by vacuum insulation; the vacuum insulation protection collet is connected with vacuum unit is evacuated to high vacuum, and the good low temperature for realizing internal cryogenic liquid is insulated and realizes that frost-free does not condense and do not influence visual inspection.The vaporizing, discharging pipe-line cell is located at the downstream of integrated glass test unit, for realizing the measurement of the controlled flow of cryogenic fluid, gasification and temperature.The present apparatus can be effectively used for the characteristic that impurity crystal grain and impurity crystal grain accumulation growth course is precipitated in dissolution, supercooling of the research soluble impurity in various cryogenic liquids.
Description
Technical field
The present invention relates to a kind of dissolutions of trace soluble impurity in cryogen engineering field more particularly to cryogenic liquid
Visual inspection device is precipitated.
Background technique
Implement in relation to dissolubility data of the soluble impurity in low-temperature solvent (liquid oxygen, liquid nitrogen) and mechanism in cryogenic engineering
It has great practical value in the process, the precipitation and accumulation of cryogenic pipe impurity in crossing cold flow is such as prevented, to avoid
The pollution of heat exchanger and pipeline, blocking and thus may caused by explosion accident.
Four oxygen are just being gradually replaced with liquid hydrogen/oxygen, liquid oxygen/kerosene or liquid oxygen/liquid methane combination cryogenic propellant
Change fuel of the conventional propellants such as phenodiazine/uns-dimethylhydrazine as big load environment-friendly type rocket of new generation.It is miscellaneous in cryogenic propellant
Quality Control fixture has higher requirements.During carrying out extensive filling cryogenic propellant for rocket pending on pylon, in propellant
Contain or the impurity components such as the water (possibility maximum), carbon dioxide, the hydrocarbon that carry are solidified at low temperature or are precipitated.
Especially rocket penetrate before add process, generally use subcooled liquid additional way, cause originally miscellaneous in dissolution equilibrium state
Matter solute is quickly precipitated.What the solid granulates of precipitation or " ice sheet " were very likely arranged in some or all of blocking infusion pipeline
Filter, or even filling is caused to fail.Solubility and Precipitation Characteristics of the impurity component in liquid oxygen is studied to help avoid conciliating
The certainly above problem.
Retrieval discovery by the prior art, about trace soluble impurity, solubility measurement is filled in cryogenic liquid at present
Existing a small amount of report is set, such as document " The high solubility of water in liquid nitrogen and
other cryogenic liquids”(Advances in Cryogenic Engineering.Springer US,1984:
A low temperature infrared absorption chamber 1005-1012) is devised for measuring water based on Fourier transformation and infrared absorption spectrum principle
Solubility in liquid nitrogen, liquid oxygen and liquid methane, for another example document " Solubility measurements for carbon
dioxide and nitrous oxide in liquid oxygen at temperatures down to 90K.
"(Fluid phase equilibria,2002,200(1):19-30) devise a static analysis device for measure 90~
110K warm area carbon dioxide, solubility of the nitrous oxide in liquid oxygen.But above-mentioned experimental provision can only realize that solubility is miscellaneous
The measurement of matter solubility in cryogenic liquid not can be carried out the visual inspection that impurity crystal grain is precipitated and gathers growth characteristics.
Therefore, those skilled in the art is dedicated to developing a kind of solution modeling of trace soluble impurity in cryogenic liquid
Solubility and Precipitation Characteristics of the impurity component in cryogenic liquid are studied in visual inspection device, help.
Summary of the invention
In view of the above drawbacks of the prior art, the technical problem to be solved by the present invention is to how design a kind of device energy
The dissolution and precipitation of visual inspection trace soluble impurity in cryogenic liquid.
To achieve the above object, the present invention provides a kind of solution modeling of trace soluble impurity in cryogenic liquid is visual
Change observation device, including integrated glass test unit (1), high speed microimaging unit (2), deep cooling solvent filling unit (3),
Soluble impurity fills unit (4), cooling medium surveys control temperature unit (5), vacuum unit (6) and vaporizing, discharging pipeline list
First (7), wherein the integration glass test unit (1) includes deep cooling solution cavity (14), cooling medium cavity (13), set
Pipe heat exchanger (16), vacuum insulation protection collet (18) and leakage fluid dram glass flange (19), the deep cooling solution cavity
(14) it is connected to respectively with the entrance of the internal and external channel of described sleeve pipe formula heat exchanger (16) with the cooling medium cavity (13)；It is described
The outlet extending section of the interior journey pipe of double pipe heat exchanger (16) is connect with the leakage fluid dram glass flange (19), and described sleeve pipe formula is changed
Draw cooling medium delivery pipe (17) in the outer shell outlet of hot device (16)；Vacuum insulation protection collet (18) coaxially covers institute
State deep cooling solution cavity (14), cooling medium cavity (13), double pipe heat exchanger (16) and its outlet extending section；The deep cooling is molten
Pass through solid glass between vacuum insulation protection collet (18) at liquid cavity (14) and the cooling medium cavity (13)
Bar (15) is connected；The vacuum insulation protective case (18) is equipped with vacuum orifice (110)；The deep cooling solution cavity (14) and institute
It states cooling medium cavity (13) and is respectively provided with the first sealing cover (11) and the second sealing cover (12)；On second sealing cover (12)
It is connect equipped with crossing cabin fluid hose with the first connector air-tightness of a four-way ferrule fitting (111)；Four-way ferrule fitting (111)
Second connector extension connection one check valve (112)；Deep cooling solvent filling unit (3) is by solvent tank (31), shut-off valve
(32) it is sequentially connected in series with flexible infusion line；Four-way ferrule fitting on the outlet end of flexible infusion line and the second sealing cover (12)
(111) third connector connection；Soluble impurity filling unit (4) is by syringe pump (41), shut-off valve (42) and silicone tube
It is sequentially connected in series；The outlet end of silicone tube is connected with the 4th connector of four-way ferrule fitting (111) on sealing cover (12).
Further, described sleeve pipe formula heat exchanger (16) is made of two coaxial nested transparent glass tubes, display pipe
(113) both ends and interior journey pipe (114) are closed, and shell-side confined space is formed；There are inflow entrance (115) and stream on display pipe (113)
It exports (116), is connected to respectively with the cooling medium cavity (13) and cooling medium delivery pipe (17)；Interior journey pipe (114)
Entrance be connected to deep cooling solution cavity (14), outlet extending section is connect with leakage fluid dram glass flange (19).
Further, the outlet extending section of journey pipe (114) is configured as downstream expander and forms a step in the glass
Face (117)；Filter screen (118) are set on the step surface (117)；Filter screen (118) is in elastic spring (119), four
The tight pipe (120) of fluorine branch, stainless steel pressure spring (121) three compound action under pre-tighten and fix.
Further, the cooling medium surveys control temperature unit (5) by micro thermocouple (51), flow control valve (52), ratio
Example integral derivative controller PLC (55) and cooling medium composition；Cooling medium is from cooling medium storage tank (56) and passes through
The pipeline being connected in series by shut-off valve (57) and four fluorine tube being connected with the crossing cabin fluid hose on the first sealing cover (11) enters set
The shell side of pipe heat exchanger (16)；Flow control valve (52) are housed on the discharge pipe of the cooling medium storage tank (56)；It is micro-
Type thermocouple (51) is installed on the interior journey pipe (114) near filter screen Nei.
Further, the PLC (55) receives the signal of micro thermocouple (51), exports control signal to flow control valve
(52) and it is executed by it the flow for controlling cooling medium.
Further, the vacuum unit (6) includes molecular pump high vacuum unit (61), metal bellows and KF flange
The vacuum gauge connector (62) of interface；Vacuum gauge connector (62) and the glass on the integrated glass test unit (1)
The connection of vacuum orifice (110) air-tightness.
Further, the vaporizing, discharging pipe-line cell (7) includes glass piping, glass flange (19), Hough epoxy method
Blue (71), metal flange (75), threeway ferrule fitting (76), cryogenic globe valve (77), air-cooled heat exchanger (78), flow are adjusted
Needle-valve (79), flowmeter (710)；The glass flange (19), the Hough epoxy flange (71), institute on the glass piping
It states metal flange (75) three combination and is equipped with expansion tetrafluoro washer realization glass to the switching of the transition seal of metal.
Further, deep cooling solution is vaporizated into gas at normal temperature after air-cooled heat exchanger (78) heat exchange, by the stream
Meter (710) measures mass flow, and records data by data collecting instrument (81) and the computer (82).
Further, the high speed microimaging unit (2) is made of high speed camera (21) and microlens (22), described
High speed microimaging unit (2) is configured as the high speed imaging to micron particles, and the computer (82) is configured as manipulating
And image recording.
Further, the lens location of the high speed microimaging unit (2) be configured in double pipe heat exchanger (16) and
It is between its inner tube outlet extension and adjustable.
The solution modeling visual inspection device of trace soluble impurity has following in cryogenic liquid of the present invention
Advantage：
(1) deep cooling solvent filling unit, soluble impurity filling unit are held with deep cooling solution by four-way ferrule fitting
Chamber is connected, and so as to realize the high-purity preparation of deep cooling sample solution, avoids being mixed into for introduced contaminants.
(2) core of this experimental observation system is made of transparent glass, and is integrated with double pipe heat exchanger, vacuum
Insulated heat collet solves while meeting the technical contradiction that two aspects of cryogen thermal insulation and visualization require.
(3) filter screen is embedded in integrated glass test unit, realizes the cryogen to reality containing impurity
The visual Simulation of filter process is subcooled.
(4) signal that sample solution temperature measured by micro thermocouple is received with PLC exports control signal and gives flow tune
Section valve and the flow for being executed by it control cooling medium obtain not to realize the automatic and accurate temperature control to deep cooling solution example
Same sample solution degree of supercooling.
(5) pipeline after transparent glass experimental provision is transitioned into metal tubes by Hough epoxy flange, therefore after making
Continuous pipeline system design is more convenient reliable.
(6) sample solution is become by gaseous material by heat exchanger and is passed through gas at normal temperature flowmeter again, thus avoid using
Cryogenic flow meter, so that test is more convenient, it is as a result relatively reliable.
It is described further below with reference to technical effect of the attached drawing to design of the invention, specific structure and generation, with
It is fully understood from the purpose of the present invention, feature and effect.
Detailed description of the invention
Fig. 1 is the overall structure diagram of a preferred embodiment of the present invention；
Fig. 2 is the integrated glass test cellular construction schematic diagram of a preferred embodiment of the present invention；
Fig. 3 is the assembling schematic diagram of Hough epoxy flange (71)；
Fig. 4 is the enlarged diagram of vacuum gauge connector (62) and metal flange (75) in Fig. 1；
Fig. 5 is the structure enlargement diagram of the filter screen fixing piece of a preferred embodiment of the present invention；
Fig. 6 is the structure enlargement diagram of pipe end part shown in Fig. 2；
Wherein, 1 integrated glass test unit；11 first sealing covers；12 second sealing covers；13 cooling medium cavities；14
Deep cooling solution cavity；15 solid glass rods；16 double pipe heat exchangers；17 cooling medium delivery pipes；18 vacuum insulations protect collet；
19 leakage fluid dram glass flanges；110 vacuum orifices；111 four-way ferrule fittings；112 check valves；113 display pipes；Journey pipe in 114；
115 leakage fluid dram glass flanges；117 step surfaces；118 filter screens；119 elastic springs；The tight pipe of 120 tetrafluoros branch；121 stainless steel pressures
Spring；2 high speed microimaging units；21 high speed cameras；22 microlens；3 deep cooling solvents fill unit；31 solvent tanks；32 sections
Only valve；4 soluble impurities fill unit；41 syringe pumps；42 shut-off valves；5 cooling mediums survey control temperature unit；51 micro thermocouples；
52 flow control valves；53 pagoda crossover subs；54 four fluorine tubes；55 proportional integral derivative controller PLC；56 cooling medium storage tanks；
57 shut-off valves；58 steel pipes；6 vacuum units；61 molecular pump high vacuum units；62 vacuum gauge connectors；7 vaporizing, discharging pipeline lists
Member；71 Hough epoxy flanges；72 taper counter sink steel discs；73 threaded hole steel discs；74 cross recessed countersunk head sscrews；75 metal flanges；
76 threeway ferrule fittings；77 cryogenic globe valves；78 air-cooled heat exchangers；79 flow metering pin valves；710 flowmeters；81 data are adopted
Collect instrument；82 computers；91 anchor ears；92 aluminium section bar boards.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1
This observation system includes integrated glass test unit 1, high speed microimaging unit 2, deep cooling solvent filling unit
3, soluble impurity filling unit 4, cooling medium survey control temperature unit 5, vacuum unit 6 and vaporizing, discharging pipe-line cell 7,
Impurity crystal grain is precipitated for dissolution, supercooling of the soluble impurity in various cryogenic liquids and impurity crystal grain gathers growth course
Characteristic research.
As shown in Figure 1, integrated glass test unit 1 is mounted on aluminium by two anchor ears 91 on horizontal and vertical direction
On profile plate 92, the high speed camera 21 equipped with microlens 22 is similarly installed at aluminium section bar board by three-dimensional support with adjustable
On.
As depicted in figs. 1 and 2, the outermost layer of integrated glass test unit 1 is that vacuum insulation protects collet 18, is vacuumized
Mouth is 110, and vacuum gauge connector 62 is tightened on vacuum orifice 110；KF16 flange-interface is welded in 62 bottom of vacuum gauge connector,
It is connected with the KF16 bellows on molecular pump high vacuum unit 61, to be vacuumized to vacuum insulation protection collet 18, prevents
Only frosting moisture condensation influences observation on the outermost layer glass wall of integrated glass test unit 1.
As shown in Fig. 2, integrated glass test unit 1 includes cooling medium cavity 13 and deep cooling solution cavity 14, difference
For storing sub-cooled fluid and containing the sample solution of impurity, deep cooling solution cavity 14 with it is true at cooling medium cavity 13
It is connected between empty insulated heat collet 18 by a solid glass rod 15, increases stability and intensity；Cooling medium cavity 13 is logical
The crossing cabin fluid hose crossed on the first sealing cover 11 is connected with cooling medium storage tank 56；Cooling medium is molten according to the sample containing impurity
Liquid type is selected, and sample solution is the liquid oxygen solution containing moisture impurity in the present embodiment, therefore selects liquid nitrogen or cold air
Nitrogen cools down sample solution as cooling medium；The second sealing cover 12 on deep cooling solution cavity 14 be equipped with crossing cabin fluid hose with
The first connector air-tightness connection of one four-way ferrule fitting 111；The second connector extension connection one of four-way ferrule fitting 111 is single
To valve 112；Cooling medium is flowed into double pipe heat exchanger 16 through cooling medium cavity 13 and is cooled down to sample solution, and from set
17 outflow of pipe heat exchanger outlet；Double pipe heat exchanger outlet 17 is inserted in one end of four fluorine tube 54, and is sealed using low temperature glue, separately
One end is then connected with pagoda crossover sub 53；By pagoda crossover sub 53, tetrafluoro tube transitions are 8mm stainless steel tube, and
One flow control valve 52 is installed, stainless steel tube thereafter is then directly communicated with environment on stainless steel tube；Double pipe heat exchanger 16 is set
It is to allow cooling medium full of entire interlayer in upper purpose that import, which is calculated as, in lower outlet, to make full use of heat exchanging interlayer table
Area reinforces heat exchange efficiency；Double pipe heat exchanger exports 17 bottoms and also is provided with vacuum protection, and the purpose is to prevent glass contact portion
Point it is thermally conductive make horizontal pipe outer wall frosting moisture condensation influence visualization.All vacuum protection sets are all communicated as one.Bushing type is changed
When cooling medium in hot device 16 is cold air nitrogen, the flow of cold air nitrogen can be adjusted by flow control valve 52, to make sample
Product solution obtains different degree of supercoolings；When the cooling fluid in double pipe heat exchanger 16 is liquid nitrogen, then flow tune need to be only closed
Valve 52 is saved, stops being filled with for liquid nitrogen after liquid nitrogen is full of double pipe heat exchanger.
Deep cooling solvent filling unit 3 as shown in Figure 1 is sequentially connected in series by solvent tank 31, shut-off valve 32 and flexible infusion line
Composition.The outlet end of flexible infusion line is connect with the third connector of four-way ferrule fitting 111 on the second sealing cover 12, thus with depth
Cold soln cavity 14 is connected to；Soluble impurity shown in FIG. 1 filling unit 4 by syringe pump 41, shut-off valve 42 and silicone tube successively
It is composed in series.The outlet end of silicone tube is connected with the 4th connector of four-way ferrule fitting 111 on the second sealing cover 12, thus with depth
Cold soln cavity 14 is connected to；Rate is filled with by what adjustable cut-off valve 32 can control solvent oxygen；The of four-way ferrule fitting 111
Two connectors extension one check valve 112 of connection, controls the pressure in the central tube of integrated glass test unit 1, prevents because filling
It is excessively high and damage to glass device to enter oxygen pressure；Oxygen is filled in the central tube of integrated glass test unit 1 simultaneously
Cold air nitrogen gradually cooling liquid in quilt cover pipe heat exchanger 16, in the process, the effect due to check valve 112 is to guarantee
Pressure in sample specimens pipeline is not too high, to ensure that the safe and reliable of device；Reach experiment to liquid oxygen amount to be taken,
It is filled with water impurity ingredient by syringe pump 41, to prepare the liquid oxygen sample solution for containing only water impurity.
By increasing the flow of cooling fluid in double pipe heat exchanger 16, further prepared sample solution is subcooled in cooling,
Sample solution after supercooling flows through at the pipeline step surface 117 for placing filter screen 118；Filter screen 118 passes through two steel wires
The fixed tetrafluoro that is coated on of retaining ring 119 props up on tight pipe 120, and stainless steel pressure spring 121 is filled in from sample solution pipe end mouth, and is passed through
Metal flange 75 is fixed tetrafluoro and props up tight pipe 120；The micro thermocouple 51 on 121 top of stainless steel pressure spring that is fastened is measured
The temperature of incoming flow sample solution.
The sample solution pipe end outward flanging of integrated glass test unit 1 forms leakage fluid dram glass flange 19, uses
In being connected and fixed two pieces of Hough epoxy flanges 71 by M6 bolt and nut with metal flange 75, two pieces of Hough epoxy flanges 71 are logical
The steel disc 73 crossed the steel disc 72 for being provided with taper counter sink and be provided with threaded hole is fixed together with cross recessed countersunk head sscrew 74；
It is compressed and is sealed with expansion tetrafluoro washer on metal flange 75 and 19 contact surface of leakage fluid dram glass flange；75 center weld of metal flange
The stainless steel tube of piece 1/4 inch diameter, so that glass pipe be made to be transitioned into metallic conduit in order to the subsequent of sample solution
Processing.
The stainless steel tube being welded on metal flange 75 is connected with threeway ferrule fitting 76.76 Vertical Square of threeway ferrule fitting
Upward interface is 51 conductor gateway of micro thermocouple, and micro thermocouple conducting wire passes through the steel pipe of an outer diameter 3mm, length 25mm
58, and steel pipe both ends are sealed, steel pipe 58 is then tightened on the ferrule fitting in 76 vertical direction of threeway ferrule fitting, miniature heat
Galvanic couple 51 is fastened on 121 top of stainless steel pressure spring, and micro thermocouple conducting wire then passes through sample solution pipeline from threeway cutting ferrule
Interface in 76 vertical direction of connector is connected with external data Acquisition Instrument 81, and finally reads temperature on computer 82 and show
Number；Stainless steel tube and 77 input end of a cryogenic globe valve connection picked out from the interface in 76 horizontal direction of threeway ferrule fitting,
The flow of liquid sample solution is controlled by cryogenic globe valve 77；The stainless steel tube of 77 outlet end of cryogenic globe valve connection passes through card
Bell and spigot joint is connected to the inlet pipeline of air-cooled heat exchanger 78,78 outlet conduit of heat exchanger by cutting ferrule again with stainless steel tube phase
Even, sample solution will become room temperature gaseous material after flowing through heat exchanger 78；Thereafter stainless steel tube is connect with flow metering pin valve 79,
The flow of the control gaseous sample solution of flow metering pin valve 79；Stainless steel tube that another exit of flow metering pin valve 79 picks out with
710 arrival end of flowmeter connection, flowmeter 710 can then measure the mass flow of gaseous sample substance and with 81 phase of data collecting instrument
Connection finally reads flowmeter registration on computer 82；710 outlet end of flowmeter equally connect a stainless steel tube directly with the external world
Environmental communication, the then sample for becoming gaseous material are directly discharged in environment, when needing to analyze sample solution ingredient,
Can also analysis detection be carried out with the sample gas constituents of sampler bag acquisition discharge herein.
It places near at the pipeline step surface 117 of filter screen 118, it is molten to flow through the sample after double pipe heat exchanger 16 is subcooled
The precipitation of impurity crystal grain will be had in liquid, and during flow further downstream, impurity crystal grain builds up filter screen 118
On.The capture that high speed camera 21 equipped with microlens 22 carries out video image to the position is acquired, and on computer 82
Observe the video image taken.Speed, the size, shape that the impurity crystal grain being specifically included under different degree of supercoolings and flow is precipitated
The movement accumulation process characteristic etc. of shape and impurity crystal grain in filter screen.
The user of the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid of the present invention
Method includes：
Vacuum insulation protection collet 18 is vacuumized：Before being tested using this observation system, to prevent integration
The outermost layer glass wall frosting of glass test unit 1 condenses, and needs first to vacuumize vacuum insulation protection collet 18.The bottom of by
The vacuum gauge connector 62 of portion's welding KF16 interface is tightened on the vacuum orifice 110 on integrated glass test unit 1, then
The KF16 flange that the bellows of KF16 interface on molecular pump high vacuum unit 61 is welded with 62 bottom of vacuum gauge connector is connect
Mouth is tightly connected by KF16 clip；When to prevent from vacuumizing, deformation occurs causes to integrated glass test unit 1 for bellows
The bellows of KF16 interface need to be fixed on aluminium section bar board by damage by clip.Molecular pump high vacuum unit 61 is exhausted with vacuum
After the 18 safety connection of Thermal protection collet, the valve on molecular pump is opened, vacuum insulation protection collet 18 is vacuumized, to true
Reciprocal of duty cycle reaches 10-5The valve on molecular pump is closed after Pa magnitude, and closes molecular pump high vacuum unit 61.
The filling of sample solution and cooling fluid：Before cooling fluid filling, cryogenic globe valve 77, flow tune can be first opened
Markingoff pin valve 79 opens shut-off valve 32 for solvent oxygen and is passed through deep cooling solution cavity 14.It is after oxygen is passed through a period of time, sample is molten
Original air discharge in liquid pipe road, then can close cryogenic globe valve 77, flow metering pin valve 79；Flow control valve 52 is opened,
Cold air nitrogen is passed through in double pipe heat exchanger 16, and finally the pipeline after double pipe heat exchanger outlet 17 is discharged into atmosphere；
The cold air nitrogen of constant flow carries out cooling liquid to the oxygen in sample solution pipeline in double pipe heat exchanger 16, in this process
In, adjustable cut-off valve 32, which controls, is filled with the rate of oxygen, check valve 112 guarantee the pressure in sample solution pipeline it is not too high and
Integrated glass test unit 1 is damaged；Reach experiment to liquid oxygen amount to be taken, closes shut-off valve 32, and pass through injection
Pump injection water impurity ingredient, to prepare the liquid oxygen sample solution for containing only water impurity.
Obtain the sample solution of different degree of supercoolings：Flow by increasing cooling fluid in double pipe heat exchanger 16 can be into one
Step is cooling to be subcooled prepared sample solution, and PLC55 receives the signal of micro thermocouple 51, exports control signal and adjusts to flow
Valve 52 and the flow for being executed by it control cooling medium, to realize the temperature control to deep cooling solution example, obtaining has different mistakes
The sample solution of cold degree；When cooling fluid is liquid nitrogen, since the temperature of liquid nitrogen under certain pressure is kept constant, therefore available one
The sample solution of the constant degree of supercooling of group.
The adjusting of sample solution flow：According to the registration of the flowmeter 710 read from computer 82, ended by low temperature
The flow of sample solution can be adjusted in valve 77, flow metering pin valve 79；One cryogenic globe valve is installed in 78 upstream of heat exchanger
77 purpose is to preferably control the sample solution of liquid.
The use of Video Image Collecting System Based：It is made into, is managed using transparent glass since integrated glass test unit 1 is whole
By the sample solution that can above observe any position.Impurity is precipitated in order to observe the impurity being dissolved in liquid oxygen solution supercooling
Crystal grain and its aggregation properties in filter screen, therefore be nearby more at the pipeline step surface 117 of placement filter screen 118
Suitable observation area.And can the parameters such as precipitation shape to crystal grain, size, speed and movement aggregation properties quantitatively divided
Analysis.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that the ordinary skill of this field is without wound
The property made labour, which according to the present invention can conceive, makes many modifications and variations.Therefore, all technician in the art
Pass through the available technology of logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Scheme, all should be within the scope of protection determined by the claims.
Claims (10)
1. the solution modeling visual inspection device of trace soluble impurity in a kind of cryogenic liquid, which is characterized in that including one
Body glass test unit (1), high speed microimaging unit (2), deep cooling solvent filling unit (3), soluble impurity filling are single
First (4), cooling medium survey control temperature unit (5), vacuum unit (6) and vaporizing, discharging pipe-line cell (7), wherein described one
Body glass test unit (1) includes deep cooling solution cavity (14), cooling medium cavity (13), double pipe heat exchanger (16), true
Empty insulated heat collet (18) and leakage fluid dram glass flange (19), the deep cooling solution cavity (14) and the cooling medium are held
Chamber (13) is connected to the entrance of the internal and external channel of described sleeve pipe formula heat exchanger (16) respectively；Described sleeve pipe formula heat exchanger (16) it is interior
The outlet extending section of journey pipe is connect with the leakage fluid dram glass flange (19), the display pipe outlet of described sleeve pipe formula heat exchanger (16)
It draws cooling medium delivery pipe (17)；Vacuum insulation protection collet (18) coaxially cover the deep cooling solution cavity (14),
Cooling medium cavity (13), double pipe heat exchanger (16) and its outlet extending section；The deep cooling solution cavity (14) with it is described cold
But it is connected between vacuum insulation protection collet (18) at medium cavity (13) by solid glass rod (15)；The vacuum
Insulated heat collet (18) is equipped with vacuum orifice (110)；The deep cooling solution cavity (14) and the cooling medium cavity
(13) the first sealing cover (11) and the second sealing cover (12) are respectively provided with；Second sealing cover (12) is equipped with crossing cabin fluid hose
It is connect with the first connector air-tightness of a four-way ferrule fitting (111)；Second connector of four-way ferrule fitting (111), which extends, to be connected
Connect a check valve (112)；Deep cooling solvent filling unit (3) is by solvent tank (31), shut-off valve (32) and flexible infusion
Pipe is sequentially connected in series；The outlet end of flexible infusion line and the third of four-way ferrule fitting (111) on the second sealing cover (12) connect
Head connection；Soluble impurity filling unit (4) is sequentially connected in series by syringe pump (41), shut-off valve (42) and silicone tube；
The outlet end of silicone tube is connected with the 4th connector of four-way ferrule fitting (111) on sealing cover (12).
2. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as described in claim 1, special
Sign is, described sleeve pipe formula heat exchanger (16) is made of two coaxial nested transparent glass tubes, the both ends of display pipe (113) with
Interior journey pipe (114) closing, forms shell-side confined space；There are inflow entrance (115) and outflux (116) on display pipe (113), respectively
It is connected to the cooling medium cavity (13) and cooling medium delivery pipe (17)；The entrance and deep cooling of interior journey pipe (114) are molten
Liquid cavity (14) connection, outlet extending section are connect with leakage fluid dram glass flange (19).
3. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as described in claim 1, special
Sign is that the outlet extending section of journey pipe (114) is configured as downstream expander and forms a step surface (117) in the glass；?
Filter screen (118) are set on the step surface (117)；Filter screen (118) is in elastic spring (119), the tight pipe of tetrafluoro branch
(120), it pre-tightens and fixes under the compound action of stainless steel pressure spring (121) three.
4. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as described in claim 1, special
Sign is that the cooling medium surveys control temperature unit (5) by micro thermocouple (51), flow control valve (52), proportional integral derivative
Controller PLC (55) and cooling medium composition；Cooling medium is from cooling medium storage tank (56) and by sealing with first
The pipeline sleeve pipe formula heat exchanger being connected in series by shut-off valve (57) and four fluorine tube that the crossing cabin fluid hose covered on (11) is connected
(16) shell side；Flow control valve (52) are housed on the discharge pipe of the cooling medium storage tank (56)；Micro thermocouple
(51) it is installed on the interior journey pipe (114) near filter screen Nei.
5. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as claimed in claim 4, special
Sign is that the PLC (55) receives the signal of micro thermocouple (51), exports control signal to flow control valve (52) and by it
Execute the flow of control cooling medium.
6. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as described in claim 1, special
Sign is that the vacuum unit (6) includes the vacuum of molecular pump high vacuum unit (61), metal bellows and KF flange-interface
Regulate connector (62)；Vacuum gauge connector (62) and the glass vacuum orifice on the integrated glass test unit (1)
(110) air-tightness is connected to.
7. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as described in claim 1, special
Sign is that the vaporizing, discharging pipe-line cell (7) includes glass piping, glass flange (19), Hough epoxy flange (71), metal
Flange (75), threeway ferrule fitting (76), cryogenic globe valve (77), air-cooled heat exchanger (78), flow metering pin valve (79), stream
Meter (710)；The glass flange (19), the Hough epoxy flange (71), the metal flange on the glass piping
(75) three's combination is equipped with expansion tetrafluoro washer and realizes that glass is transferred to the transition seal of metal.
8. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as claimed in claim 7, special
Sign is that deep cooling solution is vaporizated into gas at normal temperature after air-cooled heat exchanger (78) heat exchange, is surveyed by the flowmeter (710)
Mass flow is measured, and records data by data collecting instrument (81) and computer (82).
9. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as described in claim 1, special
Sign is that the high speed microimaging unit (2) is made of high speed camera (21) and microlens (22), and the high speed is micro- to be taken the photograph
Picture unit (2) is configured as the high speed imaging to micron particles, and computer (82) is configured as manipulation and image recording.
10. the solution modeling visual inspection device of trace soluble impurity in cryogenic liquid as claimed in claim 9, special
Sign is that the lens location of the high speed microimaging unit (2) is configured in double pipe heat exchanger (16) and its inner tube outlet
It is between extension and adjustable.
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| CN107328811A (en) * | 2017-08-28 | 2017-11-07 | 重庆科技学院 | A kind of burnt melting crystal stove of high temperature copolymerization and its temperature measuring apparatus |
| CN109030519B (en) * | 2018-06-15 | 2020-11-17 | 义乌市研创工业设计有限公司 | Operable observation recording device for cryoendoscope |
| CN109709138A (en) * | 2018-12-29 | 2019-05-03 | 北京卫星环境工程研究所 | The test macro and test method of vacuum and low temperature Frost deposit |
| CN110057821B (en) * | 2019-04-16 | 2021-09-07 | 上海交通大学 | Low-temperature microscopic imaging system for human gamete rapid freeze-thawing process observation |
| CN111879809B (en) * | 2020-06-10 | 2021-08-20 | 中国原子能科学研究院 | Method for measuring and calculating dilution times of reaction liquid in research of crystal nucleation rate |
| CN112730505B (en) * | 2020-12-18 | 2022-05-17 | 上海交通大学 | Visual experiment chamber for throttling and quantitative measurement of cryogenic fluid |
| CN112763369A (en) * | 2020-12-31 | 2021-05-07 | 中国原子能科学研究院 | Experimental device for impurity heterogeneous crystallization in sodium |
| CN113044250B (en) * | 2021-03-04 | 2022-10-18 | 上海交通大学 | Filling method based on spontaneous combustion fuel transfer and filling system |
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