CN208700568U - Purification device of ultrapure hydrogen in polycrystalline silicon production - Google Patents
Purification device of ultrapure hydrogen in polycrystalline silicon production Download PDFInfo
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- CN208700568U CN208700568U CN201821329027.5U CN201821329027U CN208700568U CN 208700568 U CN208700568 U CN 208700568U CN 201821329027 U CN201821329027 U CN 201821329027U CN 208700568 U CN208700568 U CN 208700568U
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 255
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 255
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 236
- 238000000746 purification Methods 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 49
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 145
- 238000001179 sorption measurement Methods 0.000 claims abstract description 125
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 74
- 239000007788 liquid Substances 0.000 claims abstract description 42
- 229920005591 polysilicon Polymers 0.000 claims abstract description 31
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 20
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 27
- 238000010521 absorption reaction Methods 0.000 claims description 15
- 229910052763 palladium Inorganic materials 0.000 claims description 15
- 230000003197 catalytic effect Effects 0.000 claims description 12
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 12
- 230000008676 import Effects 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 9
- 239000001307 helium Substances 0.000 claims description 8
- 229910052734 helium Inorganic materials 0.000 claims description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 8
- 238000002309 gasification Methods 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 5
- 238000001514 detection method Methods 0.000 abstract description 11
- 238000004458 analytical method Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 23
- 239000003463 adsorbent Substances 0.000 description 21
- 239000012535 impurity Substances 0.000 description 21
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 12
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 239000001301 oxygen Substances 0.000 description 12
- 238000003860 storage Methods 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000006392 deoxygenation reaction Methods 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229960004424 carbon dioxide Drugs 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 230000002000 scavenging effect Effects 0.000 description 3
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
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- 230000000694 effects Effects 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 239000003344 environmental pollutant Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
Landscapes
- Separation By Low-Temperature Treatments (AREA)
Abstract
The utility model belongs to the technical field of the purification of hydrogen in the polycrystalline silicon production, a purification device of ultrapure hydrogen in the polycrystalline silicon production is related to. The utility model discloses a purification device of ultrapure hydrogen in polysilicon production, which comprises a deaerator and a hydrogen super-purification device, wherein a low-temperature heat exchanger and a plurality of adsorption tanks connected in series are arranged in the hydrogen super-purification device, and the adsorption tanks connected in series are soaked in liquid nitrogen; the inlet of the deaerator is connected with an air inlet pipeline of raw material hydrogen, the outlet of the deaerator is connected with a low-temperature heat exchanger, and the low-temperature heat exchanger is connected with the adsorption tank; the adsorption tank is provided with a hydrogen outlet pipeline, and the hydrogen outlet pipeline of the adsorption tank is connected in parallel with a pipeline provided with a hydrogen online detection and analysis device. The utility model discloses can improve hydrogen purification's purity, reduce hydrogen super-purification's cost simultaneously to the device equipment is simple, and the cost is lower, moves reliable and stable, and the product purity stability that obtains is good.
Description
Technical field
The utility model belongs to the technical field of purification of hydrogen in production of polysilicon, in particular to a kind of polysilicon
The purification devices of ultra-pure hydrogen in production.
Background technique
Hydrogen is one of production electronic-grade polycrystalline silicon process important source material, is mainly used for the cold hydrogen of production of polysilicon
Change, CVD reduction, reduction tail gas treating unit.The purity of hydrogen directly affects the quality of the electronic-grade polycrystalline silicon product of production, with
The development of electronics industry, increasingly higher demands also proposed to the purity of hydrogen, the hydrogen purity used now via
4N, 5N rise to 6N or more.Since electronic-grade polycrystalline silicon is a kind of product of high-purity, so guaranteeing that its production institute is required
The purity of raw hydrogen be vital.
Currently, the technique and device of hydrogen purification mainly utilize catalysis reaction method, palldium alloy diffusion method, metal hydride
The designs such as partition method, pressure swing adsorption method, low-temperature adsorption.Wherein, it is catalyzed reaction method, is to make catalyst using palladium or platinum, it will
Oxygen in hydrogen is reacted with hydrogen in the presence of a catalyst generates water, then by after molecular sieve dehydration, available
The hydrogen of purity 99.999%.Pressure-variable adsorption (PSA) technology is with specific adsorbent (porosu solid substance) interior surface pair
Based on the physical absorption of gas molecule, easily adsorbs high boiling component at the same pressure using adsorbent, is not easy to adsorb low boiling
Unstripped gas, is passed through absorption by the characteristic for putting adsorbance reduction under adsorbance increase, low pressure under component and high pressure under a certain pressure
Bed, reaches the separation of hydrogen and impurity composition.Palladium membrane separation process is one of membrane separation process, is hydrogen molecule at a certain temperature
It is dissociated into hydrogen atom in palladium film side, palladium is dissolved in and is diffused into the other side, then in conjunction at molecule；It is available through level-one separation
The hydrogen of 99.99%-99.9999% purity.Low temperature processing is that cryogenic condensation is based on hydrogen and other gas boiling point differences are big
Principle remove all high boiling components other than hydrogen at the operational and be condensed into the separation method of liquid, use this side
The purity for the hydrogen that method obtains can achieve 6N or more.
Above several hydrogen purification methods are common several methods in hydrogen purification production process, but are being applied to electricity
In sub- level polysilicon production process there are the following problems:
It is catalyzed reaction method, using the hydrogen that this method is dry, the oxygen in hydrogen can only be removed, and do not can be removed in hydrogen
Other impurities, so being unable to satisfy the needs of electronic-grade polycrystalline silicon production.Pressure swing adsorption method, pressure-variable adsorption can be net on a large scale
Change hydrogen, and to the purity requirement of raw hydrogen not high (40% or more), but utilizes the hydrogen purity of pressure swing adsorption purge
It is lower, it is not able to satisfy the needs of electronic-grade polycrystalline silicon production.Palladium membrane separation process involves great expense since Metal Palladium belongs to noble metal,
And oxygen, water, heavy hydrocarbon etc. be easy to cause the damage of palladium film；Under the production status of extensive electronic-grade polycrystalline silicon, this method is simultaneously
Be not suitable for.
In consideration of it, special propose the utility model.
Utility model content
The purpose of this utility model is to provide a kind of purification devices of ultra-pure hydrogen in production of polysilicon, can be improved hydrogen
The purity of gas purification, while reducing the cost of hydrogen ultrapureization, and the appliance arrangement is simple, and cost is relatively low, it is stable can
It leans on, obtained product purity stability is good.
To achieve the above object, the technical solution adopted in the utility model are as follows:
One aspect according to the present utility model, the utility model provide a kind of purifying of ultra-pure hydrogen in production of polysilicon
Device, including oxygen-eliminating device and hydrogen super purification devices are provided with cryogenic heat exchanger and multiple concatenated in the super purification devices of hydrogen
Adsorption tanks, multiple concatenated adsorption tanks are immersed in liquid nitrogen；
The import of oxygen-eliminating device and the admission line of raw hydrogen connect, and the outlet of oxygen-eliminating device is connect with cryogenic heat exchanger, low
Warm heat exchanger is connect with adsorption tanks；
Hydrogen outlet pipeline is provided on adsorption tanks, one in parallel exists equipped with hydrogen on the hydrogen outlet pipeline of adsorption tanks
The pipeline of line detection and analysis device.
As further preferred technical solution, oxygen-eliminating device is catalytic deoxidation device, is equipped with palladium catalyst in catalytic deoxidation device.
As further preferred technical solution, hydrogen on-line checking analytical equipment is the analysis of online helium ionized gas phase chromatographic
Instrument.
As further preferred technical solution, the quantity of concatenated adsorption tanks is 3~5.
As further preferred technical solution, safety valve is equipped on the admission line of raw hydrogen.
As further preferred technical solution, liquid nitrogen exchanges heat with the hydrogen entered in adsorption tanks, and the liquid nitrogen of gasification is logical
Cross the discharge of nitrogen exhausting pipeline.
As further preferred technical solution, adsorption tanks include the first adsorption tanks, N adsorption tanks and setting in the first absorption
At least one adsorption tanks between tank and N adsorption tanks, the bottom end of the raw hydrogen outlet and the first adsorption tanks of cryogenic heat exchanger
The ultra-pure hydrogen outlet of connection, N adsorption tanks is connect with the ultra-pure hydrogen import of cryogenic heat exchanger, the ultra-pure hydrogen of cryogenic heat exchanger
Gas outlet is connect with hydrogen unit.
It further include nitrogen heater as further preferred technical solution, the nitrogen heater passes through pipeline and hydrogen
Super purification devices connection.
It further include vacuum pump as further preferred technical solution, the vacuum pump passes through pipeline and the ultrapure makeup of hydrogen
Set connection.
It further include the multiple spare absorption being in parallel with the concatenated adsorption tanks as further preferred technical solution
Tank.
Compared with prior art, the utility model has the beneficial effects that:
Raw hydrogen is first delivered to oxygen-eliminating device and carries out deoxygenation, then by the purification devices of the ultra-pure hydrogen of the utility model
Cooling down into cryogenic heat exchanger to raw hydrogen, the hydrogen after cooling, which enters to, to be filled in the adsorption tanks of adsorbent,
And adsorption tanks are immersed in liquid nitrogen, to provide low temperature environment, so that the gas of higher is inhaled in hydrogen at low ambient temperatures
Attached dose of absorption；After absorption, ultrapureization hydrogen is directly entered after the detection of hydrogen on-line checking analytical equipment is qualified
With hydrogen unit without entering hydrogen-holder, the secondary pollution of hydrogen is avoided；It is hereby achieved that nitrogen, oxygen, carbon monoxide, two
Carbonoxide, methane and the extremely low ultra-pure hydrogen of moisture content, and product purity is stablized, the purity of ultra-pure hydrogen can achieve 7N and
More than, meet the production requirement of electronic-grade polycrystalline silicon.The advantages of simple technological process, easy to operate, easy to implement, controlling party
Just.
The satisfiable processing tolerance of the purification devices of the utility model is 10-300Nm3/ H, stable and reliable operation, together
When also have operating cost low, the characteristics of equipment investment is few, easy to operate, easy maintenance, high reliablity, application easy to spread.
Detailed description of the invention
It, below will be right in order to illustrate more clearly of specific embodiment of the present invention or technical solution in the prior art
Specific embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, it is described below
In attached drawing be that some embodiments of the utility model are not paying creativeness for those of ordinary skill in the art
Under the premise of labour, it is also possible to obtain other drawings based on these drawings.
Fig. 1 is that the purification devices structure of ultra-pure hydrogen in a kind of production of polysilicon that embodiment provides of the utility model is shown
It is intended to.
Icon: 1- oxygen-eliminating device；The super purification devices of 2- hydrogen；3- cryogenic heat exchanger；4- adsorption tanks；5- liquid nitrogen storage tank；
6- raw hydrogen storage tank；7- nitrogen inlet；8- nitrogen heater；9- hydrogen on-line checking analytical equipment；10- ultra-pure hydrogen
Gas outlet conduit；11- nitrogen exhausting pipeline；12- hydric safe valve exhausting pipeline；13- liquid nitrogen outlet conduit；14- vacuum
Pump；15- vacuumizes outlet.
Specific embodiment
The technical solution of the utility model is clearly and completely described below, it is clear that described embodiment is this
Utility model a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the utility model protection
Range.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " is pacified
Dress ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally
Connection；It can be mechanical connection, be also possible to be electrically connected；Can be directly connected, can also indirectly connected through an intermediary,
It can be the connection inside two elements.For the ordinary skill in the art, above-mentioned art can be understood with concrete condition
The concrete meaning of language in the present invention.
The technical solution of the utility model is clearly and completely described below, it is clear that described embodiment is this
Utility model a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the utility model protection
Range.
It is in the description of the present invention, it should be noted that term " center ", "upper", "lower", "left", "right", " perpendicular
Directly ", the orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, and is only
For ease of description the utility model and simplify description, rather than the device or element of indication or suggestion meaning must have it is specific
Orientation, be constructed and operated in a specific orientation, therefore should not be understood as limiting the present invention.In addition, term " the
One ", " second ", " third " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " is pacified
Dress ", " connected ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or integrally
Connection；It can be mechanical connection, be also possible to be electrically connected；Can be directly connected, can also indirectly connected through an intermediary,
It can be the connection inside two elements.For the ordinary skill in the art, above-mentioned art can be understood with concrete condition
The concrete meaning of language in the present invention.
The utility model provides a kind of purification process of ultra-pure hydrogen in production of polysilicon, packet at least one embodiment
Include following steps:
Raw hydrogen, which is introduced into oxygen-eliminating device, carries out deoxygenation, enters back into cryogenic heat exchanger and cools down to raw hydrogen；
The hydrogen of cryogenic heat exchanger enters in the multiple concatenated adsorption tanks being immersed in liquid nitrogen out, by adsorption tanks
Adsorbent adsorbs the impurity in hydrogen；
A pipeline equipped with hydrogen on-line checking analytical equipment in parallel, completes to inhale on the hydrogen outlet pipeline of adsorption tanks
Attached, a small amount of hydrogen, which enters in the hydrogen on-line checking analytical equipment, to be detected, after detection is qualified, obtained ultra-pure hydrogen
It is directly entered in hydrogen unit.
The method of hydrogen ultrapureization of the utility model mainly includes three steps: (1) oxygen scavenging step, by raw hydrogen or
Raw hydrogen or the pretreated hydrogen of process are sent into oxygen-eliminating device and carry out deoxygenation, to reduce the oxygen content in raw hydrogen；(2) it drops
After completing oxygen scavenging step, raw hydrogen is sent into cryogenic heat exchanger for warm step, is carried out by cryogenic heat exchanger to raw hydrogen
Cooling, it is possible to reduce the consumption of liquid nitrogen；(3) after completing cooling step, raw hydrogen feeding is immersed in for cryogenic absorption step
In multiple concatenated adsorption tanks in liquid nitrogen, low temperature environment is provided by liquid nitrogen, at low ambient temperatures the foreign gas in hydrogen
(the higher gas of boiling point) is adsorbed the absorption of the adsorbent in tank.Ultra-pure hydrogen after completing absorption is arranged from the last one adsorption tanks
Out, and least a portion of super hydrogen after purification enters in hydrogen on-line checking analytical equipment, is analyzed and is examined by the molecular device
The impurity such as carbon monoxide, carbon dioxide, methane, nitrogen in super hydrogen after purification are surveyed, hydrogen is directly entered after detection is qualified
It is subsequent to use hydrogen storage tank without entering in hydrogen unit, it in this way can be to avoid the secondary pollution of hydrogen.
Therefore, in production of polysilicon provided by the utility model ultra-pure hydrogen purification process, first raw hydrogen is conveyed
Deoxygenation is carried out to oxygen-eliminating device, is cooled down subsequently into cryogenic heat exchanger to raw hydrogen, the hydrogen after cooling enters to dress
It is filled in the adsorption tanks of adsorbent, and adsorption tanks are immersed in liquid nitrogen, to provide low temperature environment, so that hydrogen at low ambient temperatures
The gas of middle higher is adsorbed by adsorbent；After absorption, ultrapureization hydrogen is by hydrogen on-line checking analysis dress
It is directly entered with hydrogen unit after setting detection qualification without entering hydrogen-holder, avoids the secondary pollution of hydrogen；It is hereby achieved that
Nitrogen, oxygen, carbon monoxide, carbon dioxide, methane and the extremely low ultra-pure hydrogen of moisture content, and product purity is stablized, it is ultrapure
The purity of hydrogen can achieve 7N or more, meet the production requirement of electronic-grade polycrystalline silicon.
In a preferred embodiment, the pressure of raw hydrogen be 0.8~1.2MPa, preferably 0.9~1.1MPa,
Further preferably 1.0MPa；
And/or the purity of raw hydrogen is 3~5N, preferably 4~5N, further preferably 5N；
And/or purity >=7N of obtained ultra-pure hydrogen.
The raw hydrogen of the utility model preferably comes from hydrogen high pressure storage tank pressure about 1.0MPa (10bar), purity is
5N by the pretreated hydrogen with certain purity；However be not limited to this, in actual production, can also according to operating condition,
Any other pressure is selected to be operated.
It is understood that the raw hydrogen that the utility model uses is by pretreated hydrogen or High Purity Hydrogen
Gas, source or pretreated method for raw hydrogen are not done specifically limited, such as be can be from electrolytic tank electrolysis and are passed through
Cross the high-purity hydrogen of the 5N of purifying；However be not limited to this, in actual production, above-mentioned suitable model can also be selected according to operating condition
The hydrogen of purity in enclosing is operated.
The method of the utility model can by the purity of raw hydrogen improve 1~5 order of magnitude or more than, what is obtained is ultrapure
The purity of hydrogen can achieve 7N or more, various trace impurity methane, nitrogen and water vapour etc. can be effectively removed, with tradition
Pressure-variable adsorption, catalysis reaction method etc. compare, the purity of hydrogen further significantly improves, and easy to operate, and cost is not high.It utilizes
Raw material of the hydrogen as production polysilicon after the Methods For Purification of the utility model, not only can be improved the purity of polysilicon product
And quality, and the consumption of the hydrogen in production process, energy consumption can be reduced and reduce disposal of pollutants.
In a preferred embodiment, oxygen-eliminating device is catalytic deoxidation device, is equipped with palladium catalyst in catalytic deoxidation device.
Existing catalytic deoxidation device can be used in above-mentioned oxygen-eliminating device, is equipped with metal palladium catalyst, Jin Er in catalytic deoxidation device
Under the catalysis of Metal Palladium, hydrogen is reacted with oxygen generates water, to reduce the oxygen content in raw hydrogen.
It should be noted that the utility model is not particularly limited the specific constructive form of oxygen-eliminating device, this can be used
The common any type of oxygen-eliminating device in field；The concrete operations condition of the oxygen scavenging step is also that this field is conventional, can be by this
Field technical staff regulates and controls according to the actual situation.
In a preferred embodiment, the ultra-pure hydrogen that raw hydrogen flows out in cryogenic heat exchanger and from adsorption tanks
Gas exchanges heat, and to recycle the cooling capacity of low temperature ultra-pure hydrogen, reduces the temperature of raw hydrogen and improves the outlet temperature of ultra-pure hydrogen
Degree.
In a preferred embodiment, the hydrogen flowed out from adsorption tanks, with the feed hydrogen for entering low-temperature adsorber
Gas exchanges heat, and after the ultra-pure hydrogen temperature by cold recovery reaches room temperature, is directly entered with hydrogen unit.
In cryogenic heat exchanger, raw hydrogen with from the low temperature ultra-pure hydrogen obtained after adsorbent adsorbs in adsorption tanks into
Row heat exchange, not only can be lowered into the hydrogen temperature of adsorption tanks, reduce the consumption of liquid nitrogen, can also improve outlet hydrogen
The temperature of gas, because subsequent with the hydrogen for requiring room temperature in hydrogen unit；So as to save the energy, resource consumption, drop
The production cost of low enterprise.
Described can be for example reduction apparatus, the tail gas recycling device for restoring trichlorosilane with hydrogen unit
(blowback in carbon adsorption tower regenerative process) etc..
In a preferred embodiment, the quantity of concatenated adsorption tanks be 2~6, preferably 3~5, further it is excellent
It is selected as 3；
It preferably, further include the multiple spare adsorption tanks being in parallel with the concatenated adsorption tanks；
Preferably, the temperature of adsorption bed is -192~-198 DEG C, preferably -194~-196 DEG C in adsorption tanks.
The adsorption tanks and low-temperature adsorber of the utility model are arranged in the super purification devices of hydrogen, and low-temperature adsorber is located at
The top of adsorption tanks, adsorption tanks are immersed in liquid nitrogen, and the super purification devices of hydrogen are equipped with liquid nitrogen and enter pipeline, liquid nitrogen outlet conduit
With nitrogen exhausting pipeline.
According to the utility model, the quantity of adsorption tanks in device is not done it is specifically limited, can be according to the pure of hydrogen
Degree, the condition of production of device, actual condition etc., the quantity for increasing or decreasing adsorption tanks for being suitable within the above range.As excellent
Choosing, the quantity of adsorption tanks are 3, and 3 adsorption tanks are successively connected.
What needs to be explained here is that the utility model does not do special limit for the type of the adsorbent loaded in adsorption tanks
System, can be using any reproducible adsorbent for impurity in adsorbed hydrogen commonly used in the art, such as active carbon, modification
Active carbon, molecular sieve etc.；And the adsorbent of same type is loaded in multiple adsorption tanks.
According to the utility model, multiple spare adsorption tanks can also be arranged by surpassing in hydrogen in purification devices, with above-mentioned absorption
Tank carries out parallel connection, and when so that above-mentioned adsorption tanks being in absorption mode, these spare adsorption tanks are in regeneration mode, and then improve life
Produce efficiency.
According to the utility model, the temperature of adsorption bed is -192~-198 DEG C in adsorption tanks, preferably -194~-
196℃.It is adsorbed at such a low temperature, is more advantageous to the removal of the impurity in hydrogen, adsorption effect is more preferable.
In a preferred embodiment, safety valve is equipped on the admission line of raw hydrogen；
The utility model is equipped with safety valve in hydrogen inlet pipeline, when guaranteeing that the super purification devices of hydrogen break down, protects
Demonstrate,prove present apparatus pressure in safe range.According to the utility model, Hydrogen Vapor Pressure is within the scope of 0.9~1MPa in system.
Preferably, liquid nitrogen exchanges heat with the hydrogen entered in adsorption tanks, and the liquid nitrogen of gasification is arranged by nitrogen exhausting pipeline
Out；
According to the utility model, liquid nitrogen storage enters hydrogen ultrapureization in a vertical storage tank, through conveyance conduit
In device.Surpass in purification devices in hydrogen, after liquid nitrogen and hydrogen heat exchange, the liquid nitrogen of gasification is discharged into greatly by nitrogen exhausting pipeline
Gas supplements liquid nitrogen from liquid nitrogen storage tank by automatic control circuit when liquid nitrogen drops to the lowest limit, reaches high and stops supplement in limited time.
Preferably, the hydrogen on-line checking analytical equipment is online helium ionized gas phase chromatographic analyzer.By this
Line helium ionized gas phase chromatographic analyzer can analyze CO, CO in detection hydrogen2、CH4、N2Equal impurity, detection accuracy are high.This
Utility model is not particularly limited the specific installation site of the gas chromatographicanalyzer, it is only necessary to surpass purification devices with hydrogen
It is linked together by pipeline.Preferably, the gas chromatographicanalyzer is in parallel, Er Qieqi with hydrogen outlet pipeline
The inlet pipeline of analysis of hplc instrument is smaller and has regulating valve, to guarantee that small part hydrogen enters in gas chromatographicanalyzer.
In a preferred embodiment, it is first that liquid nitrogen is ultrapure from hydrogen after the adsorbent in adsorption tanks reaches saturation
Middle discharge is set in makeup, then surpasses the nitrogen being passed through after nitrogen heater heats in purification devices to hydrogen, so that outside adsorption tanks
Side is heated and the impurity in adsorbent is desorbed, and partial impurities are vented by blow-down pipe, and remainder impurity utilizes vacuum pump
It is extracted out from adsorption tanks, completes the regeneration of adsorbent；
Preferably, the temperature of nitrogen heater is 50~85 DEG C, preferably 55~80 DEG C.
Preferably, the runing time (ultrapure working time) of the super purification devices of hydrogen was at 240 hours or so.
According to the utility model, the super purification devices of hydrogen at runtime between 240 hours or so, the adsorbent base in adsorption tanks
Originally reach saturation, need to regenerate it.For regeneration method mainly first by after liquid nitrogen therein discharge, nitrogen passes through one
After a nitrogen heater heating, after being passed through the impurity desorption that heating on the outside of adsorption tanks makes in adsorbent, partially pass through blow-down pipe
Emptying, remaining impurity are extracted out from adsorption tanks using vacuum pump, the regeneration of adsorbent are completed, with spare.
It should be understood that the content being not described in detail in the explanation of the method for above-mentioned hydrogen purification, is this field skill
The Common Parameters that art personnel are readily apparent that, therefore can be omitted detailed description thereof.
The utility model provides a kind of purification devices of ultra-pure hydrogen in production of polysilicon, packet at least one embodiment
Oxygen-eliminating device and the super purification devices of hydrogen are included, cryogenic heat exchanger and multiple concatenated adsorption tanks are provided in the super purification devices of hydrogen,
Multiple concatenated adsorption tanks are immersed in liquid nitrogen；
The import of oxygen-eliminating device and the admission line of raw hydrogen connect, and the outlet of oxygen-eliminating device is connect with cryogenic heat exchanger, low
Warm heat exchanger is connect with adsorption tanks；
Hydrogen outlet pipeline is provided on adsorption tanks, one in parallel exists equipped with hydrogen on the hydrogen outlet pipeline of adsorption tanks
The pipeline of line detection and analysis device.
The purification devices of ultra-pure hydrogen can be used to implement above-mentioned polycrystalline in production of polysilicon provided by the utility model
The purification process of ultra-pure hydrogen in silicon production.The purification devices can be improved the purity of hydrogen purification, while it is ultrapure to reduce hydrogen
The cost of change, obtained product purity stability is good, can obtain nitrogen, oxygen, carbon monoxide, carbon dioxide, methane and water
The ultra-pure hydrogen for dividing content extremely low, and product purity is stablized, the purity of ultra-pure hydrogen can achieve 7N or more, meet electron level
The production requirement of polysilicon.
The satisfiable processing tolerance of the purification devices of the utility model is 10-300Nm3/ H, stable and reliable operation, together
When also have operating cost low, the characteristics of equipment investment is few, easy to operate, easy maintenance, high reliablity, application easy to spread.
In a preferred embodiment, oxygen-eliminating device is catalytic deoxidation device, is equipped with palladium catalyst in catalytic deoxidation device；
And/or hydrogen on-line checking analytical equipment is online helium ionized gas phase chromatographic analyzer；
And/or the quantity of concatenated adsorption tanks is 2~6, preferably 3~5, further preferably 3；
And/or safety valve is equipped on the admission line of raw hydrogen,
And/or liquid nitrogen exchanges heat with the hydrogen entered in adsorption tanks, the liquid nitrogen of gasification is arranged by nitrogen exhausting pipeline
Out；
And/or adsorption tanks include the first adsorption tanks, N adsorption tanks and are arranged between the first adsorption tanks and N adsorption tanks
At least one adsorption tanks, cryogenic heat exchanger raw hydrogen outlet is connect with the bottom end of the first adsorption tanks, N adsorption tanks surpass
Pure hydrogen outlet is connect with the ultra-pure hydrogen import of cryogenic heat exchanger, and the ultra-pure hydrogen outlet of cryogenic heat exchanger connects with hydrogen unit
It connects.
It in a preferred embodiment, further include nitrogen heater and vacuum pump, the nitrogen heater and vacuum
Pump is connect by pipeline with the super purification devices of hydrogen respectively；
It and/or further include the multiple spare adsorption tanks being in parallel with the concatenated adsorption tanks.
It should be understood that the purification devices of ultra-pure hydrogen and polysilicon above-mentioned in the production of polysilicon of the utility model
The purification process of ultra-pure hydrogen is conceived based on same utility model in production, thus at least and in production of polysilicon above-mentioned
The purification process of ultra-pure hydrogen advantage having the same, the utility model repeat no more again.
It should be noted that being additionally provided with valve in the connecting pipe of each device of the utility model, equipment, such as cutting
Only valve, check-valves, ball valve, regulating valve, control valve etc., the utility model is for valve type, valve quantity, valve on each pipeline
Control etc. is not particularly limited, and can carry out selection setting according to the actual situation by those skilled in the art.
Combined with specific embodiments below and attached drawing, the utility model is described in further detail.
Embodiment 1
As shown in Figure 1, in a kind of production of polysilicon ultra-pure hydrogen purification devices, including oxygen-eliminating device 1 and hydrogen ultrapureization
Device 2 is provided with cryogenic heat exchanger 3 and multiple concatenated absorption positioned at 3 lower section of cryogenic heat exchanger in the super purification devices 2 of hydrogen
Tank 4, multiple concatenated adsorption tanks 4 are immersed in liquid nitrogen；
The import of oxygen-eliminating device 1 is connect with raw hydrogen storage tank 6 by pipeline, outlet and the cryogenic heat exchanger 3 of oxygen-eliminating device 1
Raw hydrogen import is connected by pipeline；Adsorption tanks 4 include the first adsorption tanks, N adsorption tanks and setting in the first adsorption tanks and
At least one adsorption tanks between N adsorption tanks, the raw hydrogen outlet of cryogenic heat exchanger 3 and the bottom end of the first adsorption tanks connect
It connects, the ultra-pure hydrogen outlet of N adsorption tanks is connect with the ultra-pure hydrogen import of cryogenic heat exchanger 3, the ultra-pure hydrogen of cryogenic heat exchanger 3
Gas outlet is connect with hydrogen unit；
Ultra-pure hydrogen outlet conduit 10 is provided on adsorption tanks 4, it is in parallel on the ultra-pure hydrogen outlet conduit 10 of adsorption tanks 4
One is equipped with the pipeline of hydrogen on-line checking analytical equipment 9.
Wherein, oxygen-eliminating device 1 is catalytic deoxidation device, is equipped with palladium catalyst in catalytic deoxidation device；Hydrogen on-line checking analysis dress
9 are set as online helium ionized gas phase chromatographic analyzer；The quantity of concatenated adsorption tanks 4 be 2~6, preferably 3~5, further
Preferably 3.
In addition, being equipped with safety valve on the admission line of raw hydrogen, safety valve and hydric safe valve exhausting pipeline 12 connect
It connects.
Liquid nitrogen storage tank 5 is connect by pipeline with the super purification devices 2 of hydrogen；It is connected in the bottom that hydrogen surpasses purification devices 2
Liquid nitrogen outlet conduit 13.Liquid nitrogen exchanges heat with the hydrogen entered in adsorption tanks 4, and the liquid nitrogen of gasification passes through nitrogen exhausting pipeline 11
Discharge.
Nitrogen inlet 7 is connect by pipeline with nitrogen heater 8, and nitrogen heater 8 passes through pipeline and the ultrapure makeup of hydrogen
Set 2 connections.Vacuum pump 14 is connect by pipeline with the super purification devices 2 of hydrogen；Vacuum pump 14 also with vacuumize outlet and 15 connect.
Embodiment 2
The purification process of ultra-pure hydrogen in a kind of production of polysilicon, comprising the following steps:
It is introduced into from the raw hydrogen that hydrogen high pressure storage tank pressure is about 1.0MPa, purity is 5N equipped with palladium catalyst
Deoxygenation is carried out in catalytic deoxidation device, is entered back into cryogenic heat exchanger and is cooled down to raw hydrogen；Raw hydrogen is in low-temperature heat exchange
It exchanges heat in device with the ultra-pure hydrogen flowed out from adsorption tanks, to recycle the cooling capacity of low temperature ultra-pure hydrogen, reduces raw hydrogen
Temperature and improve ultra-pure hydrogen outlet temperature；
The hydrogen of cryogenic heat exchanger enters in 3 concatenated adsorption tanks being immersed in liquid nitrogen out, by adsorption tanks
Adsorbent adsorbs the impurity in hydrogen；The temperature of adsorption bed is -194~-196 DEG C in adsorption tanks；
On the hydrogen outlet pipeline of adsorption tanks one in parallel to be equipped with hydrogen on-line checking analytical equipment helium ionized online
The pipeline of gas chromatographicanalyzer, complete absorption after, a small amount of hydrogen enter the online helium ionized gas phase chromatographic analyzer in into
Row detection, detects CO, CO in hydrogen2、CH4、N2Equal impurity, after detection is qualified, obtained ultra-pure hydrogen, which is directly entered, uses hydrogen
In unit.
Also, safety valve is equipped in hydrogen inlet pipeline and guarantees this dress when guaranteeing that the super purification devices of hydrogen break down
Set pressure in safe range.Liquid nitrogen exchanges heat with the hydrogen entered in adsorption tanks, and the liquid nitrogen of gasification passes through nitrogen blow-down pipe
Road discharge.
240 hours or so between at runtime, the adsorbent in adsorption tanks basically reaches saturation, needs to regenerate it.
Regeneration method be mainly liquid nitrogen is surpassed in purification devices from hydrogen first and is discharged, then surpass to hydrogen be passed through in purification devices by
Nitrogen after nitrogen heater heating, so that being heated on the outside of adsorption tanks and the impurity in adsorbent being desorbed, partial impurities pass through
Blow-down pipe emptying, remainder impurity extracted out from adsorption tanks using vacuum pump, is completed adsorbent and is regenerated for using.Its
In, the temperature of nitrogen heater is 55~80 DEG C.
The following table 1 gives the clean-up effect of the hydrogen of the purification process of the utility model in actual operation, ultra-pure hydrogen
It can reach 7N or more.
1 raw hydrogen of table and product hydrogen purity measurement result
| Serial number | Title | Import impurity content (PPm) | It exports impurity content (PPb) |
| 1 | N2 | < 500 | < 1 |
| 2 | O2 | < 5 | < 1 |
| 3 | CO | < 5 | < 1 |
| 4 | CO2 | < 5 | < 1 |
| 5 | CH4 | < 5 | < 1 |
| 6 | H2O | < 5 | < 1 |
From table 1 it follows that the hydrogen of the method through the utility model after purification, impurity N therein2、O2、CO、CO2、
CH4、H2O content is decreased obviously, and meets the production needs of electronic-grade polycrystalline silicon.
Finally, it should be noted that the above various embodiments is only to illustrate the technical solution of the utility model, rather than it is limited
System；Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should
Understand: it is still possible to modify the technical solutions described in the foregoing embodiments, or to some or all of
Technical characteristic is equivalently replaced；And these are modified or replaceed, it does not separate the essence of the corresponding technical solution, and this is practical new
The range of each embodiment technical solution of type.
Claims (10)
1. the purification devices of ultra-pure hydrogen in a kind of production of polysilicon, which is characterized in that including oxygen-eliminating device and the ultrapure makeup of hydrogen
It sets, cryogenic heat exchanger and multiple concatenated adsorption tanks is provided in the super purification devices of hydrogen, multiple concatenated adsorption tanks are immersed in
In liquid nitrogen；
The import of oxygen-eliminating device and the admission line of raw hydrogen connect, and the outlet of oxygen-eliminating device is connect with cryogenic heat exchanger, and low temperature changes
Hot device is connect with adsorption tanks；
It is provided with hydrogen outlet pipeline on adsorption tanks, is examined online equipped with hydrogen for one in parallel on the hydrogen outlet pipeline of adsorption tanks
Survey the pipeline of analytical equipment.
2. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that oxygen-eliminating device is to urge
Change oxygen-eliminating device, is equipped with palladium catalyst in catalytic deoxidation device.
3. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that hydrogen is examined online
Survey analytical equipment is online helium ionized gas phase chromatographic analyzer.
4. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that concatenated absorption
The quantity of tank is 3~5.
5. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that in raw hydrogen
Admission line be equipped with safety valve.
6. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that liquid nitrogen and entrance
Hydrogen in adsorption tanks exchanges heat, and the liquid nitrogen of gasification is discharged by nitrogen exhausting pipeline.
7. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that adsorption tanks include
First adsorption tanks, N adsorption tanks and at least one adsorption tanks being arranged between the first adsorption tanks and N adsorption tanks, low temperature change
The raw hydrogen outlet of hot device is connect with the bottom end of the first adsorption tanks, the ultra-pure hydrogen outlet of N adsorption tanks and cryogenic heat exchanger
Ultra-pure hydrogen import connection, cryogenic heat exchanger ultra-pure hydrogen outlet is connect with hydrogen unit.
8. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that further include nitrogen
Heater, the nitrogen heater are connect by pipeline with the super purification devices of hydrogen.
9. the purification devices of ultra-pure hydrogen in production of polysilicon according to claim 1, which is characterized in that further include vacuum
Pump, the vacuum pump are connect by pipeline with the super purification devices of hydrogen.
10. according to claim 1~9 in described in any item production of polysilicon ultra-pure hydrogen purification devices, which is characterized in that
It further include the multiple spare adsorption tanks being in parallel with the concatenated adsorption tanks.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111268646A (en) * | 2020-02-26 | 2020-06-12 | 江苏鑫华半导体材料科技有限公司 | Method and system for purifying circulating hydrogen in polycrystalline silicon production |
| CN112730791A (en) * | 2020-12-29 | 2021-04-30 | 江苏容大材料腐蚀检验有限公司 | Hydrogenation ware stainless steel build-up welding layer hydrogen peeling test system |
| CN114291791A (en) * | 2022-03-04 | 2022-04-08 | 杭州制氧机集团股份有限公司 | Device and method for preparing ultrapure hydrogen by low-temperature separation |
| CN116020250A (en) * | 2022-12-28 | 2023-04-28 | 广东省九丰氢能科技有限公司 | Hydrogen purification device in hydrolysis hydrogen production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111268646A (en) * | 2020-02-26 | 2020-06-12 | 江苏鑫华半导体材料科技有限公司 | Method and system for purifying circulating hydrogen in polycrystalline silicon production |
| CN112730791A (en) * | 2020-12-29 | 2021-04-30 | 江苏容大材料腐蚀检验有限公司 | Hydrogenation ware stainless steel build-up welding layer hydrogen peeling test system |
| CN114291791A (en) * | 2022-03-04 | 2022-04-08 | 杭州制氧机集团股份有限公司 | Device and method for preparing ultrapure hydrogen by low-temperature separation |
| CN116020250A (en) * | 2022-12-28 | 2023-04-28 | 广东省九丰氢能科技有限公司 | Hydrogen purification device in hydrolysis hydrogen production process |
| CN116020250B (en) * | 2022-12-28 | 2023-08-08 | 广东省九丰氢能科技有限公司 | Hydrogen purification device in hydrolysis hydrogen production process |
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