CN109704297A - A kind of method and device for producing solid argon by liquid nitrogen - Google Patents
A kind of method and device for producing solid argon by liquid nitrogen Download PDFInfo
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- CN109704297A CN109704297A CN201811652588.3A CN201811652588A CN109704297A CN 109704297 A CN109704297 A CN 109704297A CN 201811652588 A CN201811652588 A CN 201811652588A CN 109704297 A CN109704297 A CN 109704297A
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Abstract
The invention belongs to ultralow temperature solid preparation fields, and in particular to a kind of method and device that solid argon is produced by liquid nitrogen.The described method includes: placing step: the thermal conductive container for being placed with liquid nitrogen is placed in liquid containing argon；Vacuum step: carrying out vacuumize process to the liquid nitrogen, until the temperature of the liquid nitrogen is decreased to less than or is equal to subzero 196 DEG C, becomes super cold liquid nitrogen；The cooling liquid containing argon of super cold liquid nitrogen, obtains solid argon.Described device includes: outer barrel, outer cover, inner cylinder, inner cap body；The outer barrel and the outer cover constitute liquid cabin containing argon, and the inner cylinder and the inner cap body constitute liquid nitrogen storehouse.The present invention can make impure liquid containing argon freeze, and promote mushrooming out for solid argon (argon ice), improve preparation efficiency by obtaining super cold liquid nitrogen to liquid nitrogen vacuumize process.The present invention is simple and easy to do, low in cost, is convenient for industrialized production solid argon, is suitable for promoting the use of.
Description
Technical field
The invention belongs to ultralow temperature solid preparation fields, and in particular to a kind of method and dress that solid argon is produced by liquid nitrogen
It sets.
Background technique
Currently, most common ultralow temperature cold source is liquid nitrogen.Liquid nitrogen is harmful influence, and transport is inconvenient and at high cost, especially small
Cost is excessively high when bulk transport.When liquid nitrogen is used for ultralow temperature transportation of biological specimens, the Dewar equipped with liquid nitrogen adsorbent material is used
Tank could be used as regular general cargo to transport.This Dewar tank equipped with adsorbent material, which is called, does dry type liquid nitrogen container, liquid nitrogen adsorption process
Time is very long, is 24 hours from absorption is cooled to.It is all manual operation that liquid nitrogen, which is filled in Dewar tank, at present, and is shut out
The service life and performance of the adsorbent material of the inside of crock, which easily fail, to be not easy to hold, therefore using liquid nitrogen as ultralow temperature cold source
Higher cost, management are not easy.Liquid nitrogen is also not easy to be prepared as ultralow temperature solid, reason are as follows: and first, liquid nitrogen itself is easily formed block
Shape；Second, liquid nitrogen itself may be readily formed as liquid nitrogen slurry, but liquid nitrogen slurry is very unstable, be easy to melt.
Gu (solid that liquid argon is frozen at -189 DEG C is also known as " argon ice ", " solid argon ", " solid-state to argon block below
Argon "), finite surface area is more stable in an atmosphere, it is expected to which the convenience for becoming similar carbon dioxide dry ice (- 79 DEG C) is super
Low temperature cold source.
Normal composition of air by volume fraction at last: nitrogen (N2) accounts for about 78%, and oxygen (O2) accounts for about 21%, rare gas
Account for about 0.939%.The price of argon gas is about five times of nitrogen.Liquid oxygen, liquid nitrogen and liquid argon are using spatial division technology from air
Low-temperature liquefaction is separated and is obtained.In crude argon (liquid) before the purification of space division factory, including the concentration argon that is 97.5% and a small amount of
Oxygen and nitrogen, crude argon is by being further purified smart argon product (liquid) for 99.999%.In traditional application, steel-making is partly led
Body gas etc. needs smart argon product.But as cold source, crude argon can also be applied.
In the prior art, the method for cooling liquid argon has following two: the first is by vacuumizing: liquid argon being put into closed
In container, container connects vacuum pump；In this way, part liquid argon draw heat gasifies, remaining cooling liquid argon produces solid argon；It should
The shortcomings that method is with high costs；In addition when liquid argon is containing aerobic, nitrogen crude argon, liquid argon, liquid nitrogen, the evaporation rate of liquid oxygen are each
Not identical, engineering and solid argon ice ingredient quality are difficult to control.Second is by the heat exchange between liquid nitrogen and liquid argon: will be filled
There is the test tube of liquid argon to be put into the beaker equipped with liquid nitrogen, invisible spectro liquid argon is cooled to obtain solid argon；The disadvantages of the method are as follows
Low efficiency, speed are slow, require liquid argon purity high.If containing liquid oxygen and liquid nitrogen in liquid argon, do not allow because fusing point reduces
It is easily simple that solid argon is obtained by test tube cooling；In addition nitrogenous, oxygen containing liquid argon, fusing point can reduce, and icing then needs lower
Temperature carries out heat exchange by liquid helium and the liquid argon of low-purity under lab, expensive, is not suitable for industrialized production solid-state
Argon.
So in current scientific research and practice, need to develop it is a kind of it is low in cost, high-efficient, be suitable for industrialized production,
The method for preparing argon ice using liquid nitrogen, especially suitable for by the method for being prepared as solid argon of the crude argon containing nitrogen, oxygen impurities.It should
The solid argon that method is prepared has the convenience of dry ice (carbon dioxide of solid) carbon dioxide, can be used as new-type ultralow temperature
Dry type cold source (being less than subzero 189 DEG C) uses.
Summary of the invention
The present invention provides a kind of method and device for producing solid argon by liquid nitrogen, this method can be with low cost, height
Solid argon is prepared in efficiency, especially can will contain aerobic with low cost, high efficiency, solid-state is prepared in the crude liquid argon of nitrogen
Argon.
The present invention is realized by following technical solution:
A method of solid argon is produced by liquid nitrogen, comprising:
It places step: the thermal conductive container for being placed with liquid nitrogen is placed in liquid containing argon；Vacuum step: to the liquid nitrogen
Vacuumize process is carried out, until the temperature of the liquid nitrogen is decreased to less than or is equal to subzero 196 DEG C, becomes super cold liquid nitrogen；It is described super cold
The cooling liquid containing argon of liquid nitrogen, obtains solid argon.
As preferred embodiment, the molar content of argon element is greater than 90% in the liquid containing argon.
As preferred embodiment, one or both of nitrogen, oxygen element are also contained in the liquid containing argon；It is excellent
Selection of land, when only containing argon element, nitrogen in the liquid containing argon, the molar content of nitrogen is less than 10%, more
Preferably less than 3%；Preferably, when only containing argon element, oxygen element in the liquid containing argon, the Mole percent of oxygen element contains
Amount is less than 10% more preferably less than 3%；Preferably, when in the liquid containing argon contain argon element, nitrogen, oxygen element
When, the sum of molar content of nitrogen and oxygen element is less than 10% more preferably less than 3%.
As preferred embodiment, during the vacuumize process, nucleating agent is added into the liquid containing argon；
Preferably, the nucleating agent is dry-ice particle or ice pellets；It is highly preferred that after nucleating agent is added, the nucleating agent
The ratio between molal quantity and the molal quantity of ar atmo of molecule are less than 0.1%.
A kind of device for producing solid argon by liquid nitrogen, comprising: outer barrel, outer cover, inner cylinder, inner cap body；Wherein,
The outer barrel for holding liquid containing argon, and is equipped with thermal insulation layer and is used for internal cold insulation；The thermal insulation layer is by first
Heat-barrier material is made；The outer cover is set on the open end of the outer barrel, for closing outer barrel；The outer cover
Body is made of the second heat-barrier material；The inner cylinder is set to inside the outer barrel, for holding liquid nitrogen；The inner cylinder
It is made from a material that be thermally conductive；The inner cap body is set on the open end of the inner cylinder, for sealing the inner cylinder；Institute
Inner cap body is stated to be made of pressure-resistant material；The outer barrel and the outer cover constitute liquid cabin containing argon, the inner cylinder and described
Inner cap body constitutes liquid nitrogen storehouse.
As preferred embodiment, the liquid nitrogen storehouse is equipped with vacuum interface, for being controlled to a vacuum pump, carries out to liquid nitrogen
Vacuumize process；Preferably, the vacuum interface is set in the inner cap body.
As preferred embodiment, the liquid nitrogen storehouse is equipped with liquid nitrogen channel, enters in the inner cylinder for liquid nitrogen；It is excellent
Selection of land, the liquid nitrogen channel are set in the inner cap body；The liquid cabin containing argon is equipped with fluid passage containing argon, is used for described
Liquid containing argon is added in liquid cabin containing argon；Preferably, the fluid passage containing argon is set on outer barrel.
As preferred embodiment, the liquid cabin containing argon is equipped with nucleus channel, for being added into the outer barrel
Nucleating agent；Preferably, the nucleus channel is set on the outer barrel.
As preferred embodiment, the outer cover is arranged in the surface of the inner cap body, in the outer cover
It is provided with liquid nitrogen channel and/or vacuum interface；Liquid nitrogen channel in the outer cover is set and is arranged in the inner cap body
Liquid nitrogen channel alignment；And/or: the vacuum interface being arranged in the outer cover connects with the vacuum being arranged in the inner cap body
Mouth alignment.
The solid argon that the above method and device are produced, as ultralow temperature cold source application.
The present invention has the advantages that compared with prior art
1, the present invention is by obtaining super cold liquid nitrogen (can be down to subzero 210 DEG C), the super cold liquid to liquid nitrogen vacuumize process
Nitrogen is higher than the cooling capacity density of conventional liquid nitrogen, and the temperature difference of the liquid containing argon is big, and impure liquid containing argon can be made to freeze, and promotes solid
State argon (argon ice) mushrooms out.
2, the argon element molar content for the liquid containing argon that the present invention is used to prepare solid argon reaches 90% or more,
The liquid containing argon can not only use 99.999% smart argon product, can also greatly drop using containing aerobic and nitrogen crude argon
Low production cost.
3, the device of the invention is simple and reasonable for structure, can efficiently prepare solid argon.
4, the solid argon that is prepared of the present invention has biggish cooling capacity density, the cooling capacity compared to liquid nitrogen, in unit volume
Density is higher by about 80%, can be effective as cold source freezing and save biological sample.
5, nucleating agent is added to liquid cabin containing argon in vacuum of the invention, has further speeded up the life of solid argon
It produces.
6, the present invention is simple and easy to do, low in cost, is convenient for industrialized production solid argon, is suitable for promoting the use of.
Detailed description of the invention
Fig. 1 is the diagrammatic cross-section for the device that liquid nitrogen produces solid argon；
Fig. 2 is the diagrammatic cross-section for the device that the liquid nitrogen equipped with the fluid passage containing argon produces solid argon；
Fig. 3 is the diagrammatic cross-section for the device that the liquid nitrogen equipped with nucleus channel produces solid argon；
Fig. 4 is the diagrammatic cross-section for the device that the liquid nitrogen equipped with fluid passage containing argon, nucleus channel produces solid argon；
Fig. 5 is in working condition the diagrammatic cross-section of the device of lower Fig. 1.
Wherein: 1- outer barrel, 11- thermal insulation layer, 2- outer cover, 3- inner cylinder, 4- inner cap body, 5- vacuum interface, 6- liquid nitrogen
Channel, 7- fluid passage containing argon, 8- nucleus channel, 9- liquid levels containing argon, 10- liquid nitrogen liquid level.
Specific embodiment
In a first aspect, the present invention provides a kind of method for producing solid argon by liquid nitrogen, comprising the following steps:
Step 1: place: thermal conductive container being contained with liquid nitrogen, having cooled down is placed in liquid containing argon, liquid nitrogen and
Kept apart between liquid containing argon by thermal conductive container.
In the liquid containing argon the molar content of argon element be greater than 90% (such as: can be 90.5,91%,
92%, arbitrary value or any numberical range between the two in 93%, 94%, 95%, 96%, 97%, 98%, 99%).
The smart argon product that above-mentioned liquid containing argon can be prepared for space division factory, the molar content of argon element therein be
99.999%.
Above-mentioned liquid containing argon also may include argon element, nitrogen, oxygen element；Wherein, when only containing argon, nitrogen,
Molar content of the nitrogen in liquid containing argon be less than 10% (such as: can be 9.5%, 9%, 8%, 7%, 6%,
5%, arbitrary value or any numberical range between the two in 4%, 3%, 2%, 1%), preferably less than 3%；When only containing
When argon, oxygen element, molar content of the oxygen element in liquid containing argon be less than 10% (such as: can be 9.5%, 9%,
8%, arbitrary value or any numberical range between the two in 7%, 6%, 5%, 4%, 3%, 2%, 1%), preferably less than
3%；When containing argon, nitrogen, oxygen element simultaneously, the sum of the molar content of nitrogen and oxygen element in liquid containing argon is small
In 10% (such as: it can be arbitrary value in 9.5%, 9%, 8%, 7%, 6%, 5%, 4%, 3%, 2%, 1% or both any
Between numberical range), preferably less than 3%.The molar content of argon is higher in above-mentioned liquid containing argon, more easy to form solid
State argon；If the molar content of the molar content of oxygen element, nitrogen, or both the sum of be more than or equal to 10%,
Impurities in liquid containing argon is excessive, can not form argon ice at low temperature.
Above-mentioned liquid containing argon can be especially the crude argon (liquid) before the purification of space division factory, contain including Mole percent
Amount is 97.5% argon and a small amount of oxygen element and nitrogen.
Step 2: vacuumizing: vacuumize process is carried out to above-mentioned liquid nitrogen, until the temperature of liquid nitrogen is decreased to less than or is equal to subzero
196 DEG C, most down to subzero 210 DEG C (such as: can for -196 DEG C, -197 DEG C, -198 DEG C, -199 DEG C, -200 DEG C, -201 DEG C, -
Arbitrary value or any number between the two in 202 DEG C, -203 DEG C, -204 DEG C, -205 DEG C, -206, -208 DEG C, -20 DEG C, -210 DEG C
It is worth range), become super cold liquid nitrogen；The super cold liquid nitrogen cools down liquid containing argon, obtains solid argon.
Above-mentioned super cold liquid nitrogen is higher than the cooling capacity density of conventional liquid nitrogen, and the temperature difference of the liquid containing argon is big, can promote argon ice
It mushrooms out.
As preferred embodiment, in order to accelerate the formation speed of solid argon, improve production efficiency, this method is also wrapped
It includes:
During vacuumize process, when the temperature of liquid argon is decreased to less than or is equal to subzero 189 DEG C, to liquid containing argon
Middle addition nucleating agent, until there is solid argon to start to generate.
The mode of above-mentioned addition nucleating agent can be with are as follows: to carbon dioxide gas is passed through in liquid containing argon, by carbon dioxide gas
The dry-ice particle that body is frozen into is as nucleating agent；The volume of the carbon dioxide gas is about identical with the volume of the liquid containing argon, and two
The ratio between the molal quantity of carbon molecules and the molal quantity of ar atmo are aoxidized less than 0.1%.
The mode of above-mentioned addition nucleating agent can be with are as follows: to the argon gas containing vapor is passed through in liquid containing argon, is steamed by water
Ice pellets that gas is frozen into is as nucleating agent；Preferably, should argon gas containing vapor be the argon gas containing saturated steam (i.e.
Are as follows: vapor is mixed in the argon gas, content of the vapor in argon gas is saturation), it is somebody's turn to do the argon gas containing saturated steam
Temperature is room temperature.
After nucleating agent is added, the molal quantity of hydrone and molal quantity (that is: the ar atmo in liquid containing argon of ar atmo
With the sum of the molal quantity of ar atmo in the argon gas containing saturated steam) the ratio between less than 0.1% (for example, can for 0.08%,
0.05%, arbitrary value or any numberical range between the two in 0.03%, 0.01%, 0.005%).
Theoretically, liquid nitrogen and liquid containing argon, which pass through heat exchange, can form argon ice；But if being added without nucleating agent, then solid-state
Argon (argon ice) the formation time is long, and the speed of growth is slow.This step uses simplest inorganic nucleator --- dry ice and ice pellets, both
Can accelerate argon ice speed of production, but can to avoid other inorganic nucleators (such as: talcum powder, calcium carbonate, silica, alum,
The cheap and practical nucleating agent that titanium dioxide, calcium oxide, magnesia, carbon black, mica etc. are developed earliest) become in argon ice
Impurity, make argon ice used melt and evaporation after do not leave harmful residue.
By taking 1L as an example, under normal pressure, liquid argon becomes the refrigeration requirement of solid argon are as follows:
Q=1 × 1.398 × (0.52 × (189-186)+29.5)=43.4KJ,
The cooling capacity of IL liquid nitrogen are as follows: Q=1 × 0.837 × 200=167.4KJ,
It can be seen that the liquid argon of 1L can be prepared as argon ice by the liquid nitrogen of 1L when the thermal efficiency is 30% or so.
By the physical attribute of the gas of the following table 1 it is found that theoretically liquid helium can also prepare argon ice, but cost is excessively high.
Second aspect, as shown in Figs. 1-5, the present invention provide fill corresponding with the method for producing solid argon above by liquid nitrogen
It sets, which includes:
Outer barrel 1 is container open at one end, for holding liquid containing argon, and is equipped with thermal insulation layer 11 and is used for internal cold insulation；
Thermal insulation layer 11 is made of the first heat-barrier material.Thermal insulation layer 11 both can be set in 1 inside of outer barrel, can also be by entire outer barrel
1 is prepared with heat-barrier material, and at this moment outer barrel 1 is also equivalent to thermal insulation layer 11.First heat-barrier material can be polyolefin
Foamed material, polyurethane, aeroge or vacuum interlayer.
Outer cover 2 is set on the open end of outer barrel 1, for closing outer barrel 1 while can connect with outside atmosphere
It connects.The outer cover is made of the second heat-barrier material；Second heat-barrier material can be identical as the first heat-barrier material, can also not
It is identical, it is preferred to use high density polyolefins foamed material.
Outer barrel 1 and outer cover 2 collectively form liquid cabin containing argon.When inner cylinder 3 vacuumizes, this contains inside argon liquid cabin
Cold insulation, and can prevent air from flowing into, in case the oxygen in air liquefies in liquid containing argon influences producing for solid argon.
Inner cylinder 3 is container open at one end, is set to inside outer barrel 1, as thermal conductive container for holding liquid nitrogen；
Above-mentioned inner cylinder 2 is made of Heat Conduction Material (such as: aluminium alloy), so that the heat exchange between liquid containing argon and liquid nitrogen sufficiently carries out.
Inner cap body 4 is set on the open end of inner cylinder 3, is vacuumized for sealing inner cylinder 3；Inner cap body 4 is
It is made of pressure-resistant material, it is preferred to use aluminium alloy.
Inner cylinder 3 and inner cap body 4 collectively form liquid nitrogen storehouse, for closely holding liquid nitrogen.
Above-mentioned liquid nitrogen storehouse is equipped with vacuum interface 5, for being controlled to a vacuum pump, carries out vacuumize process to liquid nitrogen；Preferably,
Vacuum interface 5 is set in inner cap body 4.
Above-mentioned liquid nitrogen storehouse is additionally provided with liquid nitrogen channel 6, enters in inner cylinder 3 for liquid nitrogen, supplements the liquid nitrogen wherein consumed；Liquid
Nitrogen channel 6 is preferably disposed in inner cap body 4.
Above-mentioned liquid nitrogen storehouse and liquid cabin containing argon are equipped with temperature measuring equipment (such as: thermometer or temperature sensor；It is not shown), it is excellent
Choosing is set in outer cover 2 and inner cap body 4, also can be set on outer barrel 1；
It is (not shown) for deflating that above-mentioned liquid nitrogen storehouse is equipped with safety valve；It avoids that vacuum pump failure etc. occurs surprisingly in liquid nitrogen storehouse
When situation, liquid nitrogen storehouse internal pressure is excessively high, and safety valve, which is used to adjust liquid nitrogen storehouse internal pressure, maintains an atmospheric pressure.
As preferred embodiment, as shown in Figs. 1-5, above-mentioned outer cover 2 be set to be close to inner cap body 4 just on
Side, makes more compact structure；In this way, being also correspondingly provided with vacuum interface 5 and/or liquid nitrogen channel 6 in outer cover 2；It is arranged in outer cover
It is aligned between liquid nitrogen channel and the liquid nitrogen channel being arranged in inner cap body 4 on body 2, to keep the pipeline for being inserted into liquid nitrogen channel suitable
Benefit is passed through in inner cylinder 3, and/or: the vacuum interface that is arranged in outer cover 2 and the vacuum interface that is arranged in inner cap body 4 it
Between be aligned, so as to make be inserted into vacuum interface pipeline be smoothly passed through in inner cylinder 3.
As preferred embodiment, as shown in figure 3, above-mentioned liquid cabin containing argon is additionally provided with fluid passage containing argon 7, for containing
Argon liquid enters in outer barrel 1, liquid containing argon is supplemented or be added into outer barrel 1.Fluid passage containing argon 7 is preferably provided with outside
On cylinder 1.
During above-mentioned apparatus prepares solid argon, it is inserted into corresponding pipeline in vacuum interface 5, liquid nitrogen channel 6, is connect
Enter corresponding equipment (as shown in Figure 5)；After above-mentioned apparatus produces solid argon, the outer cover 2 with pipeline can be gone
It removes；Pipeline is removed from inner cap body 4 again, extra liquid nitrogen is removed from inner cylinder 3；It then will be new without channel
Outer cover 2 covers the open end in outer barrel 1, and such above-mentioned apparatus just becomes the appearance of the storage and transport applied to biological sample
Device.When the outer barrel 1 of above-mentioned apparatus is additionally provided with nucleus channel 8 and/or the fluid passage 7 containing argon, pipeline will be had by also needing to be used in
The removal of outer cover 2 and then with the channel that is set on outer barrel 1 of breather plug (such as sponge plug) closing.
As preferred embodiment, when also to carry out being added into liquid containing argon in the method that liquid nitrogen produces solid argon at
When the operation of core agent, the structure of above-mentioned apparatus, which has also been made, to be correspondingly improved:
Above-mentioned liquid cabin containing argon is additionally provided with nucleus channel 8, enters in above-mentioned outer barrel 1 for nucleating agent, to accelerate solid
The speed that argon generates；Nucleus channel 8 is set on outer barrel 1 (as shown in Figure 4).
The solid argon that the third aspect, the above method or device are produced, as ultralow temperature cold source application, in particular for saving
Biological sample.
Compared to liquid nitrogen, the cooling capacity density in the unit volume of solid argon is higher by about 80%；Reference table one,
Above-mentioned cooling capacity density calculates as follows: A liquid nitrogen cooling capacity=200 × 0.837=167.4, B solid argon cooling capacity=(162.3
+ 29.5) × 1.616=309.9；(A-B)/A=85.1%.
Principle are as follows: because the temperature difference in atmospheric conditions between liquid argon (- 186 DEG C) and solid argon (- 189 DEG C) is narrow,
The limited surface of argon ice relatively slowly, equably melts, volatilizees, rather than fast liquefying, gasification comprehensively, and institute is in order in sky
Storage and transport in gas are more suitable for the use of ultralow temperature cold source.
Table one
Note 1: the density of the solid argon of the three phase point obtained by PVT measurement solid-state and liquid argon is 1.616 ± 0.004g/
cm3.Referring to https: //www.sciencedirect.com/science/article/abs/pii/
0375960167906561。
Note 2: at 0 DEG C (32 ℉) and 1 atmospheric pressure, the density of nitrogen is 1.251 grams per liters, under 0 DEG C and 101,325kPa
The density of ultrapure nitrogen are as follows: 1,251g/L, the density at 15 DEG C is 1,185g/L.
Note 3:http: //www.r744.com/files/pdf_088.pdf.
Note 4:https: //www.engineeringtoolbox.com/carbon-dioxide-d_974.html.
Embodiment 1
The present embodiment 1 prepares solid argon using the device of Fig. 1, and preparation method includes:
(1) it is packed into liquid nitrogen into inner cylinder 3, after liquid nitrogen surface is steady, covers inner cap body 4, then essence is added into outer barrel 1
Liquid argon product；Liquid argon liquid level 7 and liquid nitrogen liquid level 8 as shown in Figure 4.
(2) outer cover 2 is covered into the open end in outer barrel 1, connects each pipeline, the liquid nitrogen in inner cylinder 3 is carried out
Vacuumize process makes the vacuum degree in inner cylinder 3 lower than 0.1 standard atmospheric pressure, and the temperature of liquid nitrogen is down to subzero 210 DEG C of formation
Super cold liquid nitrogen, until solid argon generates and growth.
The preparation method of the present embodiment compares the following prior art: the test tube equipped with sperm argon product is put into equipped with liquid nitrogen
Beaker in, invisible spectro sperm argon product is cooled to obtain solid argon；The solid argon of same weight is prepared, the present embodiment is spent
Time be only the one third of the prior art or less.
Embodiment 2
The present embodiment 1 prepares solid argon using the device of Fig. 1, and preparation method includes:
(1) it is packed into liquid nitrogen into inner cylinder 3, after liquid nitrogen surface is steady, covers inner cap body 4, then essence is added into outer barrel 1
Liquid argon product.
(2) liquid oxygen and liquid nitrogen is added into outer barrel 1 again, and is uniformly mixed, makes to form liquid containing argon in outer barrel 1,
Wherein the molar percentage of oxygen element is 5%, and the molar percentage of nitrogen is 3%.
(3) outer cover 2 is covered into the open end in outer barrel 1, connects each pipeline, the liquid nitrogen in inner cylinder 3 is carried out
Vacuumize process makes the vacuum degree in inner cylinder 3 lower than 0.1 standard atmospheric pressure, and the temperature of liquid nitrogen is down to subzero 210 DEG C of formation
Super cold liquid nitrogen, until solid argon generates and growth.
The preparation method of the present embodiment compares the following prior art: (the wherein oxygen element Mole percent of liquid containing argon will be housed
Than being 5%, nitrogen molar percentage is put into the beaker equipped with liquid nitrogen for test tube 3%), invisible spectro liquid product containing argon
It is cooled；Due to also containing nitrogen, oxygen element in liquid containing argon, so being unable to get solid argon using the prior art.
Embodiment 3
The present embodiment 1 prepares solid argon using the device of Fig. 1, and preparation method includes:
(1) it is packed into liquid nitrogen into inner cylinder 3, after liquid nitrogen surface is steady, covers inner cap body 4, then be added slightly into outer barrel 1
Argon (liquid argon before the purification of space division factory) is used as liquid containing argon, the argon for being 97.5% including molar content, and a small amount of
Oxygen and nitrogen.
(2) outer cover 2 is covered into the open end in outer barrel 1, connects each pipeline, the liquid nitrogen in inner cylinder 3 is carried out
Vacuumize process makes the vacuum degree in inner cylinder 3 lower than 0.1 standard atmospheric pressure, and the temperature of liquid nitrogen is down to subzero 210 DEG C of formation
Super cold liquid nitrogen, until solid argon generates and growth.
The preparation method of the present embodiment compares the following prior art: (the wherein oxygen element Mole percent of liquid containing argon will be housed
Than being 5%, nitrogen molar percentage is put into the beaker equipped with liquid nitrogen for test tube 3%), invisible spectro liquid product containing argon
It is cooled；Due to also containing nitrogen, oxygen element in liquid containing argon, so being unable to get solid argon using the prior art.
Embodiment 4
The present embodiment prepares solid argon using the device of Fig. 4, and preparation method includes:
(1) it is packed into liquid nitrogen into inner cylinder 3, after liquid nitrogen surface is steady, covers inner cap body 4, then essence is added into outer barrel 1
Liquid argon product.
(2) outer cover 2 is covered in outer barrel 1, connects each pipeline, the liquid nitrogen in inner cylinder 3 is carried out to vacuumize place
Reason；During vacuumize process, when the temperature of the liquid containing argon is brought down below -189 DEG C, it is passed through into outer barrel 1 a small amount of
Carbon dioxide gas (carbon dioxide gas forms dry-ice particle as nucleating agent), until there is solid argon to start to generate in outer barrel 1.
The dosage of required carbon dioxide gas is about equal with the volume of the liquid containing argon, the molal quantity of carbon dioxide molecule and ar atmo
The ratio between molal quantity is less than 0.1%.
(3) vacuum degree in inner cylinder 3 is lower than 0.1 standard atmospheric pressure, and the temperature of liquid nitrogen, which is down to subzero 210 DEG C and is formed, to be surpassed
Cold liquid nitrogen, until solid argon continues to generate and grow up.
The preparation method of the present embodiment compares the following prior art: the test tube equipped with sperm argon product is put into equipped with liquid nitrogen
Beaker in, invisible spectro sperm argon product is cooled to obtain solid argon；The solid argon of same weight is prepared, the present embodiment is spent
Time be only the prior art one third hereinafter, only embodiment 1 half.
Embodiment 5
The present embodiment prepares solid argon using the device of Fig. 4, and preparation method includes:
(1) it is packed into liquid nitrogen into inner cylinder 3, after liquid nitrogen surface is steady, covers inner cap body 4, then essence is added into outer barrel 1
Liquid argon product.
(2) outer cover 2 is covered into the open end in outer barrel 1, connects each pipeline, the liquid nitrogen in inner cylinder 3 is carried out
Vacuumize process；During vacuumize process, when the temperature of the liquid containing argon is brought down below -189 DEG C, into outer barrel 1
It is passed through a small amount of argon gas containing saturated steam (vapor forms ice pellets as nucleating agent), until thering is solid argon to open in outer barrel 1
Begin to generate.The dosage of the required argon gas containing saturated steam is about suitable with the volume of the liquid containing argon, the molal quantity of hydrone and
Ar atmo molal quantity (that is: after addition nucleus, ar atmo in liquid containing argon and the argon in the argon gas containing saturated steam
The sum of molal quantity of atom) the ratio between less than 0.1%.
(3) vacuum degree in inner cylinder 3 is lower than 0.1 standard atmospheric pressure, and the temperature of liquid nitrogen, which is down to subzero 210 DEG C and is formed, to be surpassed
Cold liquid nitrogen, until solid argon continues to generate and grow up.
The preparation method of the present embodiment compares the following prior art: the test tube equipped with sperm argon product is put into equipped with liquid nitrogen
Beaker in, invisible spectro sperm argon product is cooled to obtain solid argon；The solid argon of same weight is prepared, the present embodiment is spent
Time be only the prior art one third hereinafter, only embodiment 1 half.
It should be noted last that the above specific embodiment is only used to illustrate the technical scheme of the present invention and not to limit it,
Although being described the invention in detail referring to preferred embodiment, those skilled in the art should understand that, it can be right
Technical solution of the present invention is modified or replaced equivalently, without departing from the spirit and scope of the technical solution of the present invention,
It is intended to be within the scope of the claims of the invention.
Claims (10)
1. a kind of method for producing solid argon by liquid nitrogen, it is characterised in that: the described method includes:
It places step: the thermal conductive container for being placed with liquid nitrogen is placed in liquid containing argon；
Vacuum step: carrying out vacuumize process to the liquid nitrogen, until the temperature of the liquid nitrogen is decreased to less than or is equal to subzero 196
DEG C, become super cold liquid nitrogen；The cooling liquid containing argon of super cold liquid nitrogen, obtains solid argon.
2. method according to claim 1, it is characterised in that:
The molar content of argon element is greater than 90% in the liquid containing argon.
3. method according to claim 1, it is characterised in that:
Also contain one or both of nitrogen, oxygen element in the liquid containing argon；
Preferably, when only containing argon element, nitrogen in the liquid containing argon, the molar content of nitrogen be less than
10%, more preferably less than 3%；
Preferably, when only containing argon element, oxygen element in the liquid containing argon, the molar content of oxygen element be less than
10%, more preferably less than 3%；
Preferably, when containing argon element, nitrogen, oxygen element in the liquid containing argon, moles the hundred of nitrogen and oxygen element
Dividing the sum of content is less than 10% more preferably less than 3%.
4. any the method in -3 according to claim 1, it is characterised in that:
During the vacuumize process, nucleating agent is added into the liquid containing argon；Preferably, the nucleating agent is dry ice
Particle or ice pellets；
It is highly preferred that after nucleating agent is added, the ratio between molal quantity and the molal quantity of ar atmo of the molecule of the nucleating agent
For less than 0.1%.
5. a kind of device for producing solid argon by liquid nitrogen, it is characterised in that:
Described device includes: outer barrel, outer cover, inner cylinder, inner cap body；Wherein,
The outer barrel for holding liquid containing argon, and is equipped with thermal insulation layer and is used for internal cold insulation；The thermal insulation layer is heat-insulated by first
Material is made；
The outer cover is set on the open end of the outer barrel, for closing outer barrel；The outer cover by second every
Hot material is made；
The inner cylinder is set to inside the outer barrel, for holding liquid nitrogen；The inner cylinder is made from a material that be thermally conductive；
The inner cap body is set on the open end of the inner cylinder, for sealing the inner cylinder；The inner cap body is by resistance to
Pressure material is made；
The outer barrel and the outer cover constitute liquid cabin containing argon, and the inner cylinder and the inner cap body constitute liquid nitrogen storehouse.
6. device according to claim 5, it is characterised in that: the liquid nitrogen storehouse is equipped with vacuum interface, for connecting with vacuum pump
It connects, vacuumize process is carried out to liquid nitrogen；Preferably, the vacuum interface is set in the inner cap body.
7. device according to claim 5, it is characterised in that: the liquid nitrogen storehouse is equipped with liquid nitrogen channel, enters institute for liquid nitrogen
It states in inner cylinder；Preferably, the liquid nitrogen channel is set in the inner cap body；
The liquid cabin containing argon is equipped with fluid passage containing argon, for adding liquid containing argon into the liquid cabin containing argon；Preferably,
The fluid passage containing argon is set on outer barrel.
8. according to described device any in claim 5-7, it is characterised in that: the liquid cabin containing argon is equipped with nucleus channel, uses
In nucleating agent is added into the outer barrel；Preferably, the nucleus channel is set on the outer barrel.
9. according to claim 7 or 8 described devices, it is characterised in that: the surface of the inner cap body is arranged in the outer cover,
Liquid nitrogen channel and/or vacuum interface are also equipped in the outer cover；Liquid nitrogen channel in the outer cover and setting are set
Liquid nitrogen channel alignment in the inner cap body；And/or: the vacuum interface in the outer cover is set with setting described interior
Vacuum interface alignment on lid.
10. the solid argon that any one of any one of claim 1-4 the method or claim 5-9 described device are produced,
As ultralow temperature cold source application.
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| CN201811652588.3A CN109704297B (en) | 2018-12-29 | 2018-12-29 | Method and device for preparing solid argon through liquid nitrogen |
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Cited By (3)
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| CN110411118A (en) * | 2019-07-31 | 2019-11-05 | 上海交通大学 | A kind of ultra-low temperature cold source material and preparation method thereof |
| CN111690378A (en) * | 2020-05-28 | 2020-09-22 | 明日加加科技有限公司 | Ultralow-temperature micro-nano fluid and preparation method thereof |
| CN111854252A (en) * | 2020-07-16 | 2020-10-30 | 四川大学 | Production device and production process of optically transparent argon ice |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110411118A (en) * | 2019-07-31 | 2019-11-05 | 上海交通大学 | A kind of ultra-low temperature cold source material and preparation method thereof |
| CN111690378A (en) * | 2020-05-28 | 2020-09-22 | 明日加加科技有限公司 | Ultralow-temperature micro-nano fluid and preparation method thereof |
| CN111690378B (en) * | 2020-05-28 | 2022-06-28 | 明日加加科技有限公司 | Ultralow-temperature micro-nano fluid and preparation method thereof |
| CN111854252A (en) * | 2020-07-16 | 2020-10-30 | 四川大学 | Production device and production process of optically transparent argon ice |
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| CN109704297B (en) | 2022-06-21 |
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