CN109592640A - Hydrogen purification system and method - Google Patents
Hydrogen purification system and method Download PDFInfo
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- CN109592640A CN109592640A CN201910059404.0A CN201910059404A CN109592640A CN 109592640 A CN109592640 A CN 109592640A CN 201910059404 A CN201910059404 A CN 201910059404A CN 109592640 A CN109592640 A CN 109592640A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/52—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with liquids; Regeneration of used liquids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
- C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
- C01B2210/0017—Carbon-based materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0043—Impurity removed
- C01B2210/0045—Oxygen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses hydrogen purification systems and method.Wherein, hydrogen purification system includes: elution device, gas-liquid separation device, device for deoxidizing, cooling device, drying device, pressure-swing absorption apparatus and purifying and dedusting device.The hydrogen purification system can carry out deep purifying to hydrogen, obtain the high-purity hydrogen of 5N purity.
Description
Technical field
The present invention relates to field of metallurgy, specifically, the present invention relates to hydrogen purification systems and method.
Background technique
The chemical purity of the tungsten powder of domestic production at present is generally 3N5 (99.95%), and purity is the tungsten of 5N (99.999%)
Powder large-scale production still belongs to blank at home, and prepares an important prerequisite condition of 5N purity tungsten powder, be as raw material it
One hydrogen purity reaches 5N.In the reaction for preparing tungsten powder using hydrogen, the hydrogen usage theoretically needed is seldom, but in order to
Reaction speed and quality are improved, the pure hydrogen of excessive (10 times of theoretical amounts or so) must be used.It, need to be to reaction to reduce production cost
Remaining hydrogen carries out recycling and reusing.
However, often containing oxygen, ammonia, moisture and various granule foreigns in the hydrogen that recycling obtains, and in recycling hydrogen
In the purification process of gas, purifier apparatus is easy to introduce the impurity such as dust particles into hydrogen, influences hydrogen purity.Therefore, existing
Hydrogen purification means still have much room for improvement.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention
One purpose is to propose hydrogen purification system and method.The hydrogen purification system can carry out deep purifying to hydrogen, obtain 5N
The high-purity hydrogen of purity.
In one aspect of the invention, the invention proposes a kind of hydrogen purification systems.According to an embodiment of the invention, should
Hydrogen purification system includes: elution device, and the elution device has hydrogen outlet after hydrogen inlet and elution；Gas-liquid separation dress
It sets, hydrogen inlet is with hydrogen outlet after separation after the gas-liquid separation device has elution, hydrogen inlet and institute after the elution
Hydrogen outlet is connected after stating elution；Device for deoxidizing, the device for deoxidizing have after separation hydrogen outlet after hydrogen inlet and deoxidation,
After the separation hydrogen inlet with it is described separate rear hydrogen outlet be connected；Cooling device, the cooling device have hydrogen after deoxidation
Hydrogen outlet after gas entrance and cooling, hydrogen inlet is connected with hydrogen outlet after the deoxidation after the deoxidation；Drying device, institute
Stating drying device has hydrogen inlet and hydrogen outlet after drying after cooling, hydrogen inlet and hydrogen after the cooling after the cooling
Gas outlet is connected；Pressure-swing absorption apparatus, the pressure-swing absorption apparatus have hydrogen inlet and hydrogen outlet after absorption, institute after drying
Hydrogen inlet is connected with hydrogen outlet after the drying after stating drying；Purifying and dedusting device, the purifying and dedusting device, which has, to be inhaled
Attached hydrogen inlet and high-purity hydrogen outlet, hydrogen inlet is connected with hydrogen outlet after the absorption after the absorption.
Hydrogen purification system according to an embodiment of the present invention is drenched first with the hydrogen that elution device obtains recycling
Processing is washed, to remove the impurity such as the solid dust, the Ammonia that are mixed in hydrogen, and is cooled down to hydrogen.Cool down through elution
After hydrogen afterwards enters gas-liquid separation device progress gas-liquid separation processing, the hydrogen through crude separation enters device for deoxidizing, and passes through
Deoxidation treatment removes the oxygen being wherein mixed with.In turn, hydrogen enters cooling device after deoxidation, preliminary while by hydrogen_cooling
The moisture being wherein mixed with is removed, subsequent recycling drying device is further dried.After drying, hydrogen enters change
It is further purified in pressure adsorbent equipment, the impurity such as moisture in hydrogen, gas is further removed by adsorption treatment.Then sharp
Deep purifying carried out to hydrogen with purifying and dedusting device, removes the dust impurities being wherein mixed with, obtain meeting technique requirement at
Product hydrogen.Hydrogen purification system of the invention can carry out deep purifying to hydrogen as a result, obtain the high-purity hydrogen of 5N purity, full
Demand in sufficient 5N purity tungsten powder preparation process to hydrogen.
In addition, hydrogen purification system according to the above embodiment of the present invention can also have the following additional technical features:
In some embodiments of the invention, the hydrogen purification system further comprises: air collector, the air collector tool
There are a gas access, regeneration hydrogen inlet, fresh hydrogen entrance and gas vent, the gas access separates rear hydrogen and go out with described
Mouthful be connected, the gas vent with it is described separate rear hydrogen inlet be connected, the regeneration hydrogen inlet and the purifying and dedusting dress
The high-purity hydrogen outlet set is connected.
In some embodiments of the invention, the pressure-swing absorption apparatus includes that High Pressure Absorption unit and low pressure desorption are single
Member.It can further improve the removal effect of moisture and gaseous impurity in hydrogen as a result,.
In some embodiments of the invention, the purifying and dedusting device includes cylindrical body, hydrogen after the absorption
The side wall of the cylindrical body is arranged in entrance, and the high-purity hydrogen outlet is located at the roof of the cylindrical body；The circle
Accommodation space is defined in cylindrical body, is equipped with multiple overlay film filter cylinders in the accommodation space.It can further improve hydrogen as a result,
The removal effect of middle dust.
In some embodiments of the invention, the overlay film filter cylinder is roof-mounted BWF overlay film filter cylinder.
In some embodiments of the invention, manhole is additionally provided on the side wall of the cylindrical body.It as a result, can be further
Convenient for monitoring the operation conditions of purifying and dedusting device.
In some embodiments of the invention, back blow port is additionally provided on the roof of the cylindrical body.It as a result, can be into one
Step improves the service life of purifying and dedusting device.
In some embodiments of the invention, the purifying and dedusting device further comprises: dust discharge component, the dust discharge group
Part is located at the bottom wall of the cylindrical body, and the dust discharge component is tapered, and the top of the dust discharge component is equipped with dust-exhausting port.
In another aspect of this invention, implement the invention proposes a kind of hydrogen purification system using above-described embodiment
Hydrogen purification method.According to an embodiment of the invention, the hydrogen purification method includes: that (1) supplies hydrogen to be clean to elution
Elution processing is carried out in device, hydrogen after being eluted；(2) hydrogen after the elution is supplied into gas-liquid separation device and is carried out
Gas-liquid separation processing, hydrogen after being separated；(3) hydrogen after the separation is supplied into device for deoxidizing and carries out deoxidation treatment,
Obtain hydrogen after deoxidation；(4) hydrogen after the deoxidation is supplied into cooling device and carries out cooling treatment, hydrogen after being cooled down
Gas；(5) hydrogen after the cooling is supplied and is dried into drying device, hydrogen after being dried；It (6) will be described dry
Hydrogen, which is supplied into pressure-swing absorption apparatus, after dry carries out adsorption treatment, hydrogen after being adsorbed；(7) hydrogen after the absorption is supplied
To deep purifying processing is carried out into purifying and dedusting device, high-purity hydrogen is obtained.
Hydrogen purification method according to an embodiment of the present invention is drenched first with the hydrogen that elution device obtains recycling
Processing is washed, to remove the impurity such as the solid dust, the Ammonia that are mixed in hydrogen, and is cooled down to hydrogen.Cool down through elution
After hydrogen afterwards enters gas-liquid separation device progress gas-liquid separation processing, the hydrogen through crude separation enters device for deoxidizing, and passes through
Deoxidation treatment removes the oxygen being wherein mixed with.In turn, hydrogen enters cooling device after deoxidation, preliminary while by hydrogen_cooling
The moisture being wherein mixed with is removed, subsequent recycling drying device is further dried.After drying, hydrogen enters change
It is further purified in pressure adsorbent equipment, the impurity such as moisture in hydrogen, gas is further removed by adsorption treatment.Then sharp
Deep purifying carried out to hydrogen with purifying and dedusting device, removes the dust impurities being wherein mixed with, obtain meeting technique requirement at
Product hydrogen.Hydrogen purification method of the invention can carry out deep purifying to hydrogen as a result, obtain the high-purity hydrogen of 5N purity, full
Demand in sufficient 5N purity tungsten powder preparation process to hydrogen.
In addition, hydrogen purification system according to the above embodiment of the present invention can also have the following additional technical features:
In some embodiments of the invention, further comprise before the step (3): after by the separation hydrogen with it is described
High-purity hydrogen and fresh hydrogen are supplied to be mixed into air collector, and obtained gaseous mixture is supplied to the device for deoxidizing.
In some embodiments of the invention, reverse blowing disposal periodically is carried out to the purifying and dedusting device.It as a result, can be into one
Step improves the service life of purifying and dedusting device.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is the structural schematic diagram of hydrogen purification system according to an embodiment of the invention；
Fig. 2 is the structural schematic diagram of hydrogen purification system in accordance with another embodiment of the present invention；
Fig. 3 is the structural schematic diagram of purifying and dedusting device in hydrogen purification system according to an embodiment of the invention；
Fig. 4 is that another viewing angle constructions of purifying and dedusting device in hydrogen purification system according to an embodiment of the invention show
It is intended to；
Fig. 5 is the flow diagram of hydrogen purification method according to an embodiment of the invention；
Fig. 6 is the flow diagram of hydrogen purification method in accordance with another embodiment of the present invention.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In the description of the present invention, it is to be understood that, term " on ", "lower", "front", "rear", "top", "bottom", "inner",
The orientation or positional relationship of the instructions such as "outside" is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of describing this hair
Bright and simplified description, rather than the device or element of indication or suggestion meaning must have a particular orientation, with specific orientation
Construction and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " are used for descriptive purposes only and cannot be understood as indicating or suggesting relative importance
Or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be expressed or
Implicitly include at least one this feature.In the description of the present invention, the meaning of " plurality " is at least two, such as two, three
It is a etc., unless otherwise specifically defined.
In the present invention unless specifically defined or limited otherwise, the terms such as " installation ", " connected ", " connection ", " fixation "
It shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or is integral；It can be mechanical connection,
It is also possible to be electrically connected；It can be directly connected, can also can be inside two elements indirectly connected through an intermediary
The interaction relationship of connection or two elements, unless otherwise restricted clearly.For the ordinary skill in the art,
The specific meanings of the above terms in the present invention can be understood according to specific conditions.
In the present invention unless specifically defined or limited otherwise, fisrt feature in the second feature " on " or " down " can be with
It is that the first and second features directly contact or the first and second features pass through intermediary mediate contact.Moreover, fisrt feature exists
Second feature " on ", " top " and " above " but fisrt feature be directly above or diagonally above the second feature, or be merely representative of
First feature horizontal height is higher than second feature.
In one aspect of the invention, the invention proposes a kind of hydrogen purification systems.According to an embodiment of the invention, ginseng
Examine Fig. 1, the hydrogen purification system include: elution device 100, gas-liquid separation device 200, device for deoxidizing 300, cooling device 400,
Drying device 500, pressure-swing absorption apparatus 600 and purifying and dedusting device 700.Wherein, elution device 100 has hydrogen inlet 101
With hydrogen outlet 102 after elution；Gas-liquid separation device 200 has hydrogen inlet 201 and hydrogen outlet 202 after separation after elution,
Hydrogen inlet 201 is connected with hydrogen outlet 102 after elution after elution；Device for deoxidizing 300 is with hydrogen inlet 301 after separation and takes off
Hydrogen outlet 302 after oxygen, hydrogen inlet 301 is connected with rear hydrogen outlet 202 is separated after separation；Cooling device 400 has deoxidation
Hydrogen inlet 401 and hydrogen outlet 402 after cooling afterwards, hydrogen inlet 401 is connected with hydrogen outlet 302 after deoxidation after deoxidation；It is dry
Dry device 500 is with hydrogen outlet 502 after hydrogen inlet 501 after cooling and drying, hydrogen inlet 501 and hydrogen after cooling after cooling
Gas outlet 402 is connected；Pressure-swing absorption apparatus 600 has hydrogen inlet 601 and hydrogen outlet 602 after absorption after drying, after dry
Hydrogen inlet 601 is connected with hydrogen outlet 502 after drying；Purifying and dedusting device 700 has hydrogen inlet 701 and high-purity after absorption
Hydrogen outlet 702, hydrogen inlet 701 is connected with hydrogen outlet 602 after absorption after absorption.
Hydrogen purification system according to an embodiment of the present invention is drenched first with the hydrogen that elution device obtains recycling
Processing is washed, to remove the impurity such as the solid dust, the Ammonia that are mixed in hydrogen, and is cooled down to hydrogen.Cool down through elution
After hydrogen afterwards enters gas-liquid separation device progress gas-liquid separation processing, the hydrogen through crude separation enters device for deoxidizing, and passes through
Deoxidation treatment removes the oxygen being wherein mixed with.In turn, hydrogen enters cooling device after deoxidation, preliminary while by hydrogen_cooling
The moisture being wherein mixed with is removed, subsequent recycling drying device is further dried.After drying, hydrogen enters change
It is further purified in pressure adsorbent equipment, the impurity such as moisture in hydrogen, gas is further removed by adsorption treatment.Then sharp
Deep purifying carried out to hydrogen with purifying and dedusting device, removes the dust impurities being wherein mixed with, obtain meeting technique requirement at
Product hydrogen.Hydrogen purification system of the invention can carry out deep purifying to hydrogen as a result, obtain the high-purity hydrogen of 5N purity, full
Demand in sufficient 5N purity tungsten powder preparation process to hydrogen.
Further hydrogen purification system according to an embodiment of the present invention is described in detail below with reference to Fig. 1~4.
According to an embodiment of the invention, elution device 100 has hydrogen outlet 102 after hydrogen inlet 101 and elution, elution
Device 100 is suitable for hydrogen to be clean carrying out elution processing, so as to hydrogen after being eluted.System is purified using hydrogen of the invention
When system purifies the hydrogen recycled in tungsten powder preparation process, it will be recycled from hydrogen storage equipment first with elution device
To hydrogen eluted, to remove the impurity such as solid dust, Ammonia in hydrogen, and the hydrogen obtained to recycling drops
Temperature, in order to the progress of subsequent handling.Specific example according to the present invention, elution device can be ripe using those skilled in the art
The eluting column known, and hydrogen is eluted using water.
According to an embodiment of the invention, there is gas-liquid separation device 200 hydrogen inlet 201 after elution to go out with hydrogen after separation
Mouth 202, hydrogen inlet 201 is connected with hydrogen outlet 102 after elution after elution, hydrogen after gas-liquid separation device 200 is suitable for elute
Gas carries out gas-liquid separation processing, so as to hydrogen after being separated.Specific example according to the present invention, gas-liquid separation device can be adopted
With the moisture trap that this field is common.In some embodiments, moisture trap may be provided in elution device (such as eluting column),
After eluting column carries out elution cooling to hydrogen, air water crude separation can be directly carried out.
According to an embodiment of the invention, device for deoxidizing 300 is with hydrogen outlet after hydrogen inlet 301 after separation and deoxidation
302, hydrogen inlet 301 is connected with rear hydrogen outlet 202 is separated after separation, and hydrogen carries out after device for deoxidizing 300 is suitable for separate
Deoxidation treatment, to obtain hydrogen after deoxidation.According to an embodiment of the invention, the oxygen in hydrogen after the deoxidation that deoxidation treatment obtains
Gas content is not higher than 2 μ L/L.It should be noted that the type of device for deoxidizing is not particularly restricted, if can effectively by
Oxygen removing in hydrogen makes the oxygen content in hydrogen meet technique and requires (such as not higher than 2 μ L/L), this field skill
The deoxidation equipment that art personnel can select this field common according to actual needs.
According to an embodiment of the invention, cooling device 400 has hydrogen inlet 401 and hydrogen outlet after cooling after deoxidation
402, hydrogen inlet 401 is connected with hydrogen outlet 302 after deoxidation after deoxidation, and cooling device 400 is suitable for carrying out hydrogen after deoxidation
Cooling treatment, so as to hydrogen after being cooled down.According to an embodiment of the invention, cooling device can take the photograph hydrogen_cooling to 7~10
Family name's degree, and the moisture being mixed in hydrogen is tentatively removed while cooling.It should be noted that the type of cooling device not by
Especially limitation, as long as can be effectively by hydrogen_cooling to target temperature (such as 7~10 degrees Celsius), those skilled in the art
The cooling equipment that member can select this field common according to actual needs.
According to an embodiment of the invention, drying device 500 has hydrogen inlet 501 and hydrogen outlet after drying after cooling
502, hydrogen inlet 501 is connected with hydrogen outlet 402 after cooling after cooling, and drying device 500 is suitable for carrying out hydrogen after cooling
It is dried, so as to hydrogen after being dried.Specific example according to the present invention, drying device can be dry equipped with desiccant
The type of dry tower, desiccant is not particularly restricted, and those skilled in the art can select according to actual needs.Meanwhile
Carbon molecular sieve adsorbent be there also is provided in drying device hydrogen to be dried, so as to further increase the drying of hydrogen
Effect.
Inventors have found that in the drying process to hydrogen, since hot and cold alternation, regenerative adsorption etc. can occur for carbon molecular sieve
Physical change, effect of drying after long-time service decline, and can generate dust particles, cause the water content of hydrogen product it is not up to standard,
And it is mixed with the dust impurities of carbon molecular sieve generation.In consideration of it, hydrogen purification system of the invention is further after drying device
Pressure-swing absorption apparatus and purifying and dedusting device are set, so as to carry out adsorption treatment and deep purifying to hydrogen after drying, obtained
Obtain the hydrogen product of high-purity.
According to an embodiment of the invention, there is pressure-swing absorption apparatus 600 hydrogen inlet 601 after drying to go out with hydrogen after absorption
Mouth 602, hydrogen inlet 601 is connected with hydrogen outlet 502 after drying after drying, and pressure-swing absorption apparatus 600 is suitable for hydrogen after drying
Gas carries out adsorption treatment, so as to hydrogen after being adsorbed.Hydrogen can be forced into 1.8~2.5MPa after drying and enter pressure-variable adsorption
Device is further purified in pressure-swing absorption apparatus, make product hydrogen water content (with dew point characterize water content) not higher than-
70 degrees Celsius, foreign gas total content is not higher than 5ppm.
It should be noted that the type that pressure-variable adsorption is set is not particularly restricted, as long as can effectively be inhaled by transformation
Moisture and foreign gas, those skilled in the art in attached method removing hydrogen can select ability according to actual needs
The common pressure-swing absorption apparatus equipment in domain.According to an embodiment of the invention, pressure-swing absorption apparatus may include High Pressure Absorption unit and
Low pressure desorption unit.Specific example according to the present invention, pressure-swing absorption apparatus are pressure-swing absorber, and pressure-swing absorber uses double tower
Parallel connection, an adsorption tower are used to carry out hydrogen and impurity High Pressure Absorption, and another adsorption tower is used to carry out low pressure solution to hydrogen
It inhales, to complete the further purification to hydrogen.
According to an embodiment of the invention, purifying and dedusting device 700 has hydrogen inlet 701 and high-purity hydrogen outlet after absorption
702, hydrogen inlet 701 is connected with hydrogen outlet 602 after absorption after absorption, and purifying and dedusting device 700 is suitable for hydrogen after absorption
Deep purifying processing is carried out, to obtain high-purity hydrogen.
According to an embodiment of the invention, purifying and dedusting device 700 includes cylindrical body 710, after absorption with reference to Fig. 3 and 4
The side wall of cylindrical body 710 is arranged in hydrogen inlet 701, and high-purity hydrogen outlet 702 is located at the roof of cylindrical body 710；Circle
Accommodation space is defined in cylindrical body, is equipped with multiple overlay film filter cylinders in accommodation space.The hydrogen warp of pressure-swing absorption apparatus output
Purifying and dedusting device 700 is entered by hydrogen inlet 701 after adsorbing after surge tank decompression, and depth is carried out by hydrogen purifying part
It purifies, dust removal rate of the partial size greater than 0.5 μm is up to 99.999% in hydrogen, to obtain the hydrogen production that purity reaches 5N
Product.
According to some embodiments of the present invention, above-mentioned overlay film filter cylinder can be roof-mounted BWF overlay film filter cylinder.Specifically, more
A roof-mounted BWF overlay film filter cylinder can be mounted in parallel with each other in the accommodation space of purifying and dedusting device.Pressure-variable adsorption as a result,
After hydrogen enters the accommodation space of purifying and dedusting device after the absorption of device output, carried out by roof-mounted BWF overlay film filter cylinder deep
Degree purification then exports discharge from the high-purity hydrogen for being located at purifying and dedusting device roof, obtains high-purity hydrogen product.In some realities
It applies in example, the surface of BWF overlay film filter cylinder has expanded microporous polytetra fluoroethylene-EPTEE film, and the coefficient of friction of the film is small, and hydrophobicity is strong, clearly
Grey effect is good, is well suited for for removing the dust in hydrogen.The aperture of expanded microporous polytetra fluoroethylene-EPTEE film is 0.3 μm, in hydrogen
Dust removal rate of the partial size greater than 0.5 μm is up to 99.999%.
According to an embodiment of the invention, being additionally provided with manhole 703 on the side wall of purifying and dedusting device cylindrical body 710.By
This, can further monitor the operation conditions of purifying and dedusting device by manhole.
According to an embodiment of the invention, it is additionally provided with back blow port 704 on the roof of purifying and dedusting device cylindrical body 710,
Blowback is carried out to purifying and dedusting device 700 by 704 air inlet of back blow port, to blow the dust adsorbed in hydrogen purifying part
It falls, guarantees the normal use of hydrogen purifying part, and can be further improved the service life of purifying and dedusting device.
According to an embodiment of the invention, purifying and dedusting device 700 still further comprises dust discharge component 720.Dust discharge component 720
It is located at the bottom wall of purifying and dedusting device cylindrical body 710, dust discharge component 720 is tapered, and the top of dust discharge component 720 is equipped with
Dust-exhausting port 705.The dust collected and carrying out blowback to hydrogen purifying part as a result, can be by dust discharge component
720 discharges.Dust discharge component 720 is tapered simultaneously, thus more conducively dust-exhausting port 705 row of the dust from the top of dust discharge component 720
Out.
With reference to Fig. 2, according to an embodiment of the invention, hydrogen purification system of the invention can further include: gas collection
Tank 800.Air collector 800 has gas access 801, regeneration hydrogen inlet 802, fresh hydrogen entrance 803 and gas vent 804,
Gas access 801 is connected with rear hydrogen outlet 202 is separated, and gas vent 804 is connected with rear hydrogen inlet 301 is separated, regenerated hydrogen
Gas entrance 802 is connected with the high-purity hydrogen of purifying and dedusting device 700 outlet 702.Hydrogen by gas-liquid separation processing can be
It is mixed in air collector 800 with the fresh hydrogen of the obtained high-purity hydrogen of regeneration exported of purifying and dedusting device 700 and supplement, thus
It can achieve the purpose of the recycling and reusing of hydrogen.Specific example according to the present invention, by hydrogen after separation and regeneration hydrogen and
After fresh hydrogen mixing, gained gaseous mixture is pressurized to 10~15kPa by Roots blower, and supplies by surge tank to subsequent
Device for deoxidizing 300 in carry out deoxidation treatment.
In another aspect of this invention, implement the invention proposes a kind of hydrogen purification system using above-described embodiment
Hydrogen purification method.According to an embodiment of the invention, the hydrogen purification method includes: that (1) supplies hydrogen to be clean to elution
Elution processing is carried out in device, hydrogen after being eluted；(2) hydrogen after elution is supplied into gas-liquid separation device and carries out gas-liquid
Separating treatment, hydrogen after being separated；(3) hydrogen after separation is supplied into device for deoxidizing and carries out deoxidation treatment, obtain deoxidation
Hydrogen afterwards；(4) hydrogen after deoxidation is supplied into cooling device and carries out cooling treatment, hydrogen after being cooled down；(5) after will be cooling
Hydrogen is supplied to be dried into drying device, hydrogen after being dried；(6) hydrogen after drying is supplied to pressure-variable adsorption
Adsorption treatment is carried out in device, hydrogen after being adsorbed；(7) hydrogen after absorption is supplied and carries out depth into purifying and dedusting device
Purified treatment obtains high-purity hydrogen.
Hydrogen purification method according to an embodiment of the present invention is drenched first with the hydrogen that elution device obtains recycling
Processing is washed, to remove the impurity such as the solid dust, the Ammonia that are mixed in hydrogen, and is cooled down to hydrogen.Cool down through elution
After hydrogen afterwards enters gas-liquid separation device progress gas-liquid separation processing, the hydrogen through crude separation enters device for deoxidizing, and passes through
Deoxidation treatment removes the oxygen being wherein mixed with.In turn, hydrogen enters cooling device after deoxidation, preliminary while by hydrogen_cooling
The moisture being wherein mixed with is removed, subsequent recycling drying device is further dried.After drying, hydrogen enters change
It is further purified in pressure adsorbent equipment, the impurity such as moisture in hydrogen, gas is further removed by adsorption treatment.Then sharp
Deep purifying carried out to hydrogen with purifying and dedusting device, removes the dust impurities being wherein mixed with, obtain meeting technique requirement at
Product hydrogen.Hydrogen purification method of the invention can carry out deep purifying to hydrogen as a result, obtain the high-purity hydrogen of 5N purity, full
Demand in sufficient 5N purity tungsten powder preparation process to hydrogen.
Further hydrogen purification method according to an embodiment of the present invention is described in detail below with reference to Figures 5 and 6.According to
The embodiment of the present invention, the hydrogen purification method include:
S100: elution processing
In the step, hydrogen to be clean is supplied into elution device and carries out elution processing, hydrogen after being eluted.It utilizes
When hydrogen purification method of the invention purifies the hydrogen recycled in tungsten powder preparation process, first with elution device
It will be eluted from the hydrogen recycled with hydrogen storage equipment, to remove the impurity such as solid dust, Ammonia in hydrogen, and to returning
It receives obtained hydrogen to cool down, in order to the progress of subsequent handling.Specific example according to the present invention, elution device can be adopted
With eluting column well known to those skilled in the art, and hydrogen is eluted using water.
S200: gas-liquid separation processing
In the step, hydrogen after elution is supplied into gas-liquid separation device and carries out gas-liquid separation processing, after obtaining separation
Hydrogen.Specific example according to the present invention, the moisture trap that gas-liquid separation device can be common using this field.In some realities
It applies in example, moisture trap may be provided in elution device (such as eluting column), can be straight after eluting column carries out elution cooling to hydrogen
Tap into promoting the circulation of qi water crude separation.
S300: deoxidation treatment
In the step, hydrogen after separation is supplied into device for deoxidizing and carries out deoxidation treatment, obtains hydrogen after deoxidation.According to
The embodiment of the present invention, oxygen content is not higher than 2 μ L/L in hydrogen after the deoxidation that deoxidation treatment obtains.It should be noted that
The type of device for deoxidizing is not particularly restricted, as long as can effectively remove the oxygen in hydrogen, makes the oxygen in hydrogen
Content meets technique and requires (such as not higher than 2 μ L/L), and those skilled in the art can select ability according to actual needs
The common deoxidation equipment in domain.
S400: cooling treatment
In the step, hydrogen after deoxidation is supplied into cooling device and carries out cooling treatment, hydrogen after being cooled down.According to
The embodiment of the present invention, cooling device can be by hydrogen_cooling to 7~10 degrees Celsius, and tentatively removes in hydrogen while cooling
The moisture being mixed with.It should be noted that the type of cooling device is not particularly restricted, as long as can be effectively by hydrogen_cooling
To target temperature (such as 7~10 degrees Celsius), those skilled in the art can select according to actual needs this field common
Cooling equipment.
S500: it is dried
In the step, hydrogen after cooling is supplied and is dried into drying device, hydrogen after being dried.According to
Specific example of the invention, drying device can be the drying tower equipped with desiccant, and the type of desiccant is not particularly restricted,
Those skilled in the art can select according to actual needs.Meanwhile it there also is provided carbon molecular sieve adsorbent in drying device
Hydrogen is dried, so as to further increasing the drying effect of hydrogen.
Inventors have found that in the drying process to hydrogen, since hot and cold alternation, regenerative adsorption etc. can occur for carbon molecular sieve
Physical change, effect of drying after long-time service decline, and can generate dust particles, cause the water content of hydrogen product it is not up to standard,
And it is mixed with the dust impurities of carbon molecular sieve generation.In consideration of it, hydrogen purification method of the invention is further after drying treatment
Adsorption treatment and deep purifying processing are carried out to hydrogen, so as to carry out adsorption treatment and deep purifying to hydrogen after drying,
Obtain the hydrogen product of high-purity.
S600: adsorption treatment
In the step, hydrogen after drying is supplied into pressure-swing absorption apparatus and carries out adsorption treatment, hydrogen after being adsorbed.
Hydrogen can be forced into 1.8~2.5MPa after drying and enter pressure-swing absorption apparatus, further be mentioned in pressure-swing absorption apparatus
It is pure, make product hydrogen water content (characterizing water content with dew point) not higher than -70 degrees Celsius, foreign gas total content is not higher than
5ppm。
It should be noted that the type that pressure-variable adsorption is set is not particularly restricted, as long as can effectively be inhaled by transformation
Moisture and foreign gas, those skilled in the art in attached method removing hydrogen can select ability according to actual needs
The common pressure-swing absorption apparatus equipment in domain.According to an embodiment of the invention, pressure-swing absorption apparatus may include High Pressure Absorption unit and
Low pressure desorption unit.Specific example according to the present invention, pressure-swing absorption apparatus are pressure-swing absorber, and pressure-swing absorber uses double tower
Parallel connection, an adsorption tower are used to carry out hydrogen and impurity High Pressure Absorption, and another adsorption tower is used to carry out low pressure solution to hydrogen
It inhales, to complete the further purification to hydrogen.
S700: deep purifying processing
In the step, hydrogen after absorption is supplied into purifying and dedusting device and carries out deep purifying processing, obtains High Purity Hydrogen
Gas.The hydrogen of pressure-swing absorption apparatus output enters purifying and dedusting device by hydrogen inlet 701 after adsorbing after surge tank is depressured
700, and deep purifying is carried out by hydrogen purifying part, partial size is reachable greater than 0.5 μm of dust removal rate in hydrogen
99.999%, to obtain the hydrogen product that purity reaches 5N.
According to an embodiment of the invention, reverse blowing disposal periodically can be carried out to purifying and dedusting device, to purify hydrogen
The dust adsorbed on component is blown off, and guarantees the normal use of hydrogen purifying part, and can be further improved purifying and dedusting device
Service life.
With reference to Fig. 6, hydrogen purification method of the invention can further include before S300:
S800: hydrogen after separation is mixed with regeneration hydrogen and fresh hydrogen
In the step, high-purity hydrogen and fresh hydrogen that hydrogen after separation and regeneration obtain are supplied into air collector mixed
It closes, and obtained gaseous mixture is supplied to the device for deoxidizing.By gas-liquid separation processing hydrogen can in air collector with
The obtained high-purity hydrogen of regeneration of purifying and dedusting device output and the fresh hydrogen mixing of supplement, so as to reach returning for hydrogen
Receive the purpose recycled.The hydrogen lost in production process is supplemented by the way that fresh hydrogen is added, it is ensured that the hydrogen of production and application
Tolerance and pressure are enough.Specific example according to the present invention, after hydrogen after separation is mixed with regeneration hydrogen and fresh hydrogen,
Gained gaseous mixture is pressurized to 10~15kPa by Roots blower, and by surge tank supply into subsequent device for deoxidizing into
Row deoxidation treatment.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only to describe
Property, without limiting the invention in any way.
Embodiment
The hydrogen recycled in tungsten powder preparation process is purified using hydrogen purification system of the invention
Eluting column is initially entered from the hydrogen recycled with hydrogen storage equipment, spray removes the impurity such as solid dust, Ammonia and drops
Temperature.Hydrogen after clear water washing cooling enters cyclone separator in tower after crude separation, raw hydrogen air collector is arrived after separation
And converge the fresh hydrogen of regeneration hydrogen and supplement.After being pressurized to 10~15kPa by Roots blower, enter by surge tank
Deoxidation tower makes oxygen content in hydrogen≤2 μ L/L, carries out level-one dehumidifying subsequently into hydrogen cooler and condenser, it is cooled to 7~
10 degrees Celsius of hydrogen carries out second level into the drying tower equipped with desiccant and dries, then is forced into 1.8~2.5MPa, into
Enter pressure-swing absorber (double tower is in parallel, and an adsorption tower is used for High Pressure Absorption, and one parses for low pressure) further purification, makes to produce
Product hydrogen water content (being characterized with dew point)≤- 70 degrees Celsius, foreign gas total content are less than 5ppm, are depressured by surge tank, so
Enter afterwards from hydrogen inlet after the absorption of purifying and dedusting device, by hydrogen purifying part in device, purified hydrogen is by height
Pure hydrogen outlet discharge, wherein the dust removal rate greater than 0.5 μm is up to 99.999%, hydrogen product purity is up to 99.999%
And dew point is stablized, and product hydrogen air collector is eventually entered into, and obtains the finished hydrogen for meeting technique requirement, hydrogen purification device is regular
Blowback is carried out by back blow port air inlet, to ensure the normal use of cleaning equipment, while improving service life of equipment.
Wherein, the parameter that mouth is in charge of in the middle part of purifying and dedusting device is as shown in table 1:
Table 1
| Title | Nominal diameter | Connection(size) (dimension) standard |
| Hydrogen inlet after absorption | DN250 | PN1.6HG20592-2009 |
| High-purity hydrogen outlet | DN250 | PN1.6HG20592-2009 |
| Back blow port | DN50 | PN1.6HG20592-2009 |
| Dust-exhausting port | DN125 | PN1.6HG20592-2009 |
| Manhole | DN500 | PN1.0GB/T 9119-2000 |
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of hydrogen purification system characterized by comprising
Elution device, the elution device have hydrogen outlet after hydrogen inlet and elution；
Gas-liquid separation device, the gas-liquid separation device have hydrogen inlet and hydrogen outlet after separation, the elution after elution
Hydrogen inlet is connected with hydrogen outlet after the elution afterwards；
Device for deoxidizing, the device for deoxidizing is with hydrogen outlet after hydrogen inlet after separation and deoxidation, and hydrogen enters after the separation
Mouthful with described to separate rear hydrogen outlet connected；
Cooling device, the cooling device have hydrogen inlet and hydrogen outlet after cooling after deoxidation, and hydrogen enters after the deoxidation
Mouth is connected with hydrogen outlet after the deoxidation；
Drying device, the drying device have hydrogen inlet and hydrogen outlet after drying after cooling, and hydrogen enters after the cooling
Mouth is connected with hydrogen outlet after the cooling；
Pressure-swing absorption apparatus, the pressure-swing absorption apparatus have hydrogen inlet and hydrogen outlet after absorption, the drying after drying
Hydrogen inlet is connected with hydrogen outlet after the drying afterwards；
Purifying and dedusting device, the purifying and dedusting device has hydrogen inlet and high-purity hydrogen outlet after absorption, after the absorption
Hydrogen inlet is connected with hydrogen outlet after the absorption.
2. hydrogen purification system according to claim 1, which is characterized in that further comprise:
Air collector, the air collector have gas access, regeneration hydrogen inlet, fresh hydrogen entrance and gas vent, the gas
Body entrance separates rear hydrogen outlet and is connected with described, the gas vent and connected, the regeneration that separates rear hydrogen inlet
Hydrogen inlet is connected with the outlet of the high-purity hydrogen of the purifying and dedusting device.
3. hydrogen purification system according to claim 1, which is characterized in that the pressure-swing absorption apparatus includes High Pressure Absorption
Unit and low pressure desorption unit.
4. hydrogen purification system according to claim 1, which is characterized in that the purifying and dedusting device includes cylindrical sheet
Body, the side wall of the cylindrical body is arranged in hydrogen inlet after the absorption, and the high-purity hydrogen outlet is located at the cylinder
The roof of ontology；Accommodation space is defined in the cylindrical body, is equipped with multiple overlay film filter cylinders in the accommodation space；
Optionally, the overlay film filter cylinder is roof-mounted BWF overlay film filter cylinder.
5. hydrogen purification system according to claim 4, which is characterized in that be additionally provided on the side wall of the cylindrical body
Manhole.
6. hydrogen purification system according to claim 4, which is characterized in that be additionally provided on the roof of the cylindrical body
Back blow port.
7. hydrogen purification system according to claim 6, which is characterized in that the purifying and dedusting device further comprises:
Dust discharge component, the dust discharge component are located at the bottom wall of the cylindrical body, and the dust discharge component is tapered, and the row
The top of dirt component is equipped with dust-exhausting port.
8. a kind of hydrogen purification method implemented using the described in any item hydrogen purification systems of claim 1~7, feature are existed
In, comprising:
(1) hydrogen to be clean is supplied into elution device and carries out elution processing, hydrogen after being eluted；
(2) hydrogen after the elution is supplied into gas-liquid separation device and carries out gas-liquid separation processing, hydrogen after being separated；
(3) hydrogen after the separation is supplied into device for deoxidizing and carries out deoxidation treatment, obtain hydrogen after deoxidation；
(4) hydrogen after the deoxidation is supplied into cooling device and carries out cooling treatment, hydrogen after being cooled down；
(5) hydrogen after the cooling is supplied and is dried into drying device, hydrogen after being dried；
(6) hydrogen after the drying is supplied into pressure-swing absorption apparatus and carries out adsorption treatment, hydrogen after being adsorbed；
(7) hydrogen after the absorption is supplied into purifying and dedusting device and carries out deep purifying processing, obtain high-purity hydrogen.
9. hydrogen purification method according to claim 8, which is characterized in that further comprise before step (3):
Hydrogen after the separation is supplied into the mixing that mixes, and will obtain into air collector with the high-purity hydrogen and fresh hydrogen
Gas is supplied to the device for deoxidizing.
10. hydrogen purification method according to claim 8, which is characterized in that periodically carried out to the purifying and dedusting device
Reverse blowing disposal.
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