CN111573643A - Helium recovery and purification device and method - Google Patents

Helium recovery and purification device and method Download PDF

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Publication number
CN111573643A
CN111573643A CN202010516292.XA CN202010516292A CN111573643A CN 111573643 A CN111573643 A CN 111573643A CN 202010516292 A CN202010516292 A CN 202010516292A CN 111573643 A CN111573643 A CN 111573643A
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recovery
gas
helium
mass flow
purification
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郭会军
杨俊鹏
杨辉
陈伟
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Anhui Zhongke Wanneng Technology Co ltd
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Anhui Zhongke Wanneng Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00Noble gases; Compounds thereof
    • C01B23/001Purification or separation processes of noble gases
    • C01B23/0036Physical processing only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/047Pressure swing adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/228Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2256/00Main component in the product gas stream after treatment
    • B01D2256/18Noble gases
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0405Purification by membrane separation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042Purification by adsorption on solids
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0001Separation or purification processing
    • C01B2210/0009Physical processing
    • C01B2210/001Physical processing by making use of membranes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0001Separation or purification processing
    • C01B2210/0009Physical processing
    • C01B2210/0014Physical processing by adsorption in solids
    • C01B2210/0015Physical processing by adsorption in solids characterised by the adsorbent
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0029Obtaining noble gases
    • C01B2210/0031Helium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0029Obtaining noble gases
    • C01B2210/0032Neon

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

The invention discloses a helium recovery and purification device which comprises a recovery gas tank, a recovery compression pump, a gas membrane separator, a gas purification tower and a vacuum pump, wherein the recovery gas tank is connected with the gas membrane separator; an inlet pipeline of the recovery compression pump is connected with a recovery gas tank, a first pressure transmitter is installed on the recovery gas tank, a first mass flow controller is installed on the inlet pipeline of the recovery gas tank, and an inlet of the first mass flow controller is connected with a helium recovery scene; the outlet pipeline of the recovery compression pump is connected with the gas membrane separator, the outlet pipeline of the gas membrane separator is connected with the gas purification tower, the gas purification tower is not less than two groups, all the groups are connected in parallel, the gas flow direction of each group of gas purification tower is controlled by a control valve, the inlet pipeline of the gas purification tower is connected with the vacuum pump, and the outlet pipeline is connected with the second mass flow control meter. The invention adopts a composite method of membrane and pressure swing adsorption, can complete the recovery and purification operation of low-concentration helium, hydrogen, neon and the like under complex working conditions, and has high recovery efficiency and high purity.

Description

Helium recovery and purification device and method
Technical Field
The invention relates to a helium recovery and purification device and a method.
Background
Helium is a colorless and odorless inert gas, and is widely used in various industrial fields such as optical fiber manufacturing, semiconductor production, metal manufacturing, welding, leak detection and the like. Although the helium has wide application and large usage amount, the helium has limited sources and is a scarce strategic resource. Helium content in air is about 5ppm, has no extraction value basically, is mainly derived from associated gas recovery in natural gas exploitation at present, and meanwhile, helium is a global strategic resource, reserves are limited, and export control of main production countries is tightened day by day. Therefore, the method has great significance for recycling helium which is a scarce resource which is not suitable for obtaining.
At present, there is a patent "an on-line helium recovery and purification apparatus" (publication No. CN108328588A), which includes a recovery device and a purification device; the recovery device comprises a recovery gas tank and a vacuum pump; the purification device comprises a heat exchanger, a filter, a primary membrane separator, a secondary membrane separator and a helium concentration detector; the invention recovers helium or helium-containing mixed gas under the action of a vacuum pump, boosts the pressure of the helium or helium-containing mixed gas, removes dust and water through a heat exchanger and a filter, then passes through a membrane separator and purifies and removes impurities, detects the concentration of the helium through a helium concentration detector, supplies the helium to a mass flow meter MFC through a path A and is reused by helium equipment after reaching a set standard, returns the helium which does not reach the set standard to a recovery gas tank through a path B for secondary purification, thereby ensuring that the concentration and the impurity content of the helium after the equipment is purified reach the standard and avoiding using unqualified helium by the helium equipment. The patent only adopts a two-stage membrane separation technology (single membrane treatment mode), and the separation effect is poor.
In another patent, "a helium recovery and purification device" (publication number CN206156757U) includes a flow meter, a primary filter, a vacuum pump, a compressor, a precision filter, a first buffer tank, an adsorption system, a second buffer tank, and a cryogenic tower, which are connected in sequence; the adsorption system comprises at least 2 groups of adsorption columns which are connected in series, and at least three groups of heat exchangers which are connected in series are arranged in the cryogenic tower, so that the purity of the purified helium is more than or equal to 99.999%. This patent discloses the use of a gas adsorption column, but only for the removal of water and carbon dioxide.
Disclosure of Invention
In view of the problems in the prior art, the present invention provides a helium recovery and purification apparatus and method.
In order to achieve the purpose, the helium recovery and purification device adopted by the invention comprises a recovery gas tank, a recovery compression pump, a gas membrane separator, a gas purification tower and a vacuum pump;
an inlet pipeline of the recovery compression pump is connected with a recovery gas tank, a first pressure transmitter is installed on the recovery gas tank, a first mass flow controller is installed on the inlet pipeline of the recovery gas tank, and an inlet of the first mass flow controller is connected with a helium recovery scene;
the system comprises a recovery compression pump, a gas membrane separator, a gas purification tower, a control valve, a vacuum pump, a mass flow controller II and a control valve, wherein an outlet pipeline of the recovery compression pump is connected with the gas membrane separator, an outlet pipeline of the gas membrane separator is connected with the gas purification tower, the gas purification tower is not less than two groups, the groups are connected in parallel, the gas purification tower controls the gas flow direction through the control valve, an inlet pipeline of the gas purification tower is connected with the vacuum pump for regeneration.
As an improvement, a gas one-way valve is arranged on a pipeline between the recovery compression pump and the recovery gas tank.
And as an improvement, a second pressure transmitter is arranged on a pipeline connecting each group of gas purification towers with the second mass flow controller.
As an improvement, the recovery compression pump adopts an oil-free or oil-lubricated compressor, the recovery negative pressure of the recovery compression pump is more than or equal to 100mbar, and the outlet pressure is less than or equal to 8 bar.
As an improvement, a first pressure transmitter arranged on the recovery gas tank and a first mass flow controller arranged on the inlet pipeline are matched to realize an interlocking function, so that the negative pressure environment of the recovery gas tank is maintained.
As an improvement, any one of a molecular sieve, activated carbon or a filtering mechanism is filled in the gas purification tower, and at least one group of gas redistribution devices is arranged in each group of gas purification towers.
As an improvement, the control valve adopts any one of an electromagnetic valve, a pneumatic valve and an electric valve.
As an improvement, one of a back pressure valve, a throttle valve or an electric control proportional valve is arranged at the tail gas outlet of the gas membrane separator.
Finally, the invention also provides a recovery and purification method adopting the helium recovery and purification device, which comprises the following steps: and the used helium is recycled and enters a recycling gas tank after being metered by a mass flow controller I, the helium enters a gas membrane separator under the action of a recycling compression pump, the separated helium enters a gas purification tower under the control of a control valve, and the purified helium enters helium using equipment after being metered by a mass flow controller II.
Compared with the prior art, the invention adopts a composite method of membrane and pressure swing adsorption, can complete the recovery and purification operation of low-concentration helium, hydrogen, neon and the like under complex working conditions, can purify the recovered helium, hydrogen, neon and the like to more than 99.9 percent, has the advantages of high recovery efficiency, high purity of purified gas and the like, and effectively reduces the consumption of helium, hydrogen, neon and the like.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure: 1. the device comprises a first mass flow control meter 2, a first pressure transmitter 3, a recovery gas tank 4, a recovery compression pump 5, a gas membrane separator 6, a back pressure valve 7, a control valve 8, a vacuum pump 9, a gas purification tower 10, a second pressure transmitter 11 and a second mass flow control meter.
Detailed Description
The following examples are further illustrative of the present invention as to the technical content of the present invention, but the essence of the present invention is not limited to the following examples, and one of ordinary skill in the art can and should understand that any simple changes or substitutions based on the essence of the present invention should fall within the protection scope of the present invention.
As shown in fig. 1, a helium recovery and purification device comprises a recovery gas tank 3, a recovery compression pump 4, a gas membrane separator 5, a gas purification tower 9 and a vacuum pump 8;
an inlet pipeline of the recovery compression pump 4 is connected with a recovery gas tank 3, a first pressure transmitter 2 is installed on the recovery gas tank 3, a first mass flow controller 1 is installed on an inlet pipeline of the recovery gas tank 3, and an inlet of the first mass flow controller 1 is connected with a helium recovery scene;
the outlet pipeline of the recovery compression pump 4 is connected with the gas membrane separator 5, the outlet pipeline of the gas membrane separator 5 is connected with the gas purification tower 9, the gas purification towers 9 are not less than two groups, the groups are connected in parallel, the gas purification towers 9 of each group control the gas flow direction through the control valve 7, the inlet pipeline of the gas purification tower 9 is connected with the vacuum pump 8, the gas purification tower 9 is regenerated by the vacuum pump 8, and the outlet pipeline of the gas purification tower 9 is connected with the mass flow controller II 11.
As a modification of the embodiment, a gas check valve is arranged on a pipeline between the recovery compression pump 4 and the recovery gas tank 3 to ensure the flow direction of gas. A first mass flow controller 1 arranged on an inlet pipeline of the recycling gas tank 3 and used for measuring the amount of recycled gas, and a gas content detecting instrument arranged at the upstream or downstream of a connecting pipeline of the first mass flow controller 1 and used for detecting the components and the content of the recycled gas in real time; in addition, the mass flow controller 1 can be replaced by a flowmeter, a flow meter, a proportional solenoid valve and the like.
As a modification of the embodiment, a second pressure transmitter 10 is installed on the pipeline connecting each group of gas purifying towers 9 and a second mass flow controller 11.
As an improvement of the embodiment, the recovery compression pump 4 adopts an oil-free or oil-lubricated compressor, the recovery negative pressure of the recovery compression pump 4 is more than or equal to 100mbar, and the outlet pressure is less than or equal to 8 bar.
As an improvement of the embodiment, the first pressure transmitter 2 installed on the recovery gas tank 3 and the first mass flow controller 1 installed on the inlet pipeline are matched to realize an interlocking function, that is, when the value of the first pressure transmitter 2 is smaller, the opening degree of the first mass flow controller 1 is reduced, and when the value of the first pressure transmitter 2 is larger, the opening degree of the first mass flow controller 1 is increased, so that the purpose of real-time dynamic adjustment is achieved, the recovery gas tank 3 is maintained in a negative pressure environment with constant pressure, and the recovery efficiency is improved.
As an improvement of the embodiment, a connecting pipeline between the recovery compression pump 4 and the gas membrane separator 5 can be provided with pressure, temperature and content detecting instruments and the like; the tail gas outlet of the gas membrane separator 5 adjusts the process state of the gas membrane separator 5 through a back pressure valve 6 or a throttle valve, in addition, the back pressure valve 6 or the throttle valve can be replaced by an electric control proportional valve; the gas permeation outlet of the gas membrane separator 5 is connected to the gas purification tower 9 through a pipeline, and a pressure, temperature and content detecting instrument and the like can be arranged on the pipeline between the gas permeation outlet and the gas purification tower.
The gas purifying tower 9 can be two groups, three groups, four groups or even more groups, and the gas purifying tower 9 controls the switching and regeneration operation between the gas flow direction and the gas purifying tower by the control valves 7 with different numbers; the control valve 7 can adopt valves such as an electromagnetic valve, a pneumatic valve, an electric valve and the like.
Any one of a molecular sieve, activated carbon or a filtering mechanism is filled in the gas purifying tower 9, and at least one group of gas redistribution devices is arranged in each group of gas purifying tower 9.
And a pipeline between the gas purification tower 9 and the second mass flow controller 11 is provided with pressure, temperature and gas content detecting instruments and the like. The gas purification tower 9 used in the invention can effectively remove a series of impurities such as nitrogen, oxygen, argon, water, carbon dioxide and the like, and the gas purification tower completely works in a normal temperature environment.
Finally, the parameters and data acquisition and control in the helium recovery and purification device are controlled by a PLC, a logic circuit and the like.
The invention relates to a composite method based on membrane (adopting a high-molecular hollow fiber membrane, wherein the membrane material is usually a high-molecular polymer material such as polysulfone, polyamide and the like) and pressure swing adsorption, wherein the pressure swing adsorption means that a separated component is pressurized and adsorbed on an adsorbent in a purification tower (the purification tower is usually filled with a molecular sieve, activated carbon and the like), and then is desorbed from the adsorbent through pressure reduction. The invention adopts more than two purifying towers, namely when one purifying tower is in a desorption process, at least one other purifying tower is put into adsorption work in real time.
Example 1
By adopting the helium recovery and purification device and method, the recovery amount is 18.2L/min, the content of the recovered helium is 38.0 percent (the balance is air), the helium with the purity of 99.9 percent can be produced after the helium is pressurized by the recovery compression pump 4, separated by the hollow fiber membrane separator and purified by the gas purification tower 9, the gas amount after purification is 6.8L/min, and the purification rate of the whole device and the process method is calculated to be more than 98 percent (the calculation method is 6.8 x 0.999/(18.2 x 0.38)). The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (9)

1. The helium recovery and purification device is characterized by comprising a recovery gas tank (3), a recovery compression pump (4), a gas membrane separator (5), a gas purification tower (9) and a vacuum pump (8);
an inlet pipeline of the recovery compression pump (4) is connected with a recovery gas tank (3), a first pressure transmitter (2) is installed on the recovery gas tank (3), a first mass flow controller (1) is installed on an inlet pipeline of the recovery gas tank (3), and an inlet of the first mass flow controller (1) is connected with a helium recovery scene;
the gas purification device is characterized in that an outlet pipeline of the recovery compression pump (4) is connected with the gas membrane separator (5), an outlet pipeline of the gas membrane separator (5) is connected with the gas purification tower (9), the gas purification tower (9) is not less than two groups, all the groups are connected in parallel, each group of gas purification tower (9) controls the gas flow direction through the control valve (7), an inlet pipeline of the gas purification tower (9) is connected with the vacuum pump (8) for regeneration, and an outlet pipeline is connected with the mass flow control meter II (11).
2. The helium recovery and purification device as claimed in claim 1, wherein a gas check valve is installed on the pipeline between the recovery compression pump (4) and the recovery gas tank (3).
3. The helium recovery and purification device as claimed in claim 1, wherein a second pressure transmitter (10) is installed on the pipeline connecting each group of gas purification towers (9) and the second mass flow controller (11).
4. The helium recovery and purification device of claim 1, wherein the recovery compression pump (4) adopts an oil-free or oil-lubricated compressor, the recovery negative pressure of the recovery compression pump (4) is not less than 100mbar, and the outlet pressure is not more than 8 bar.
5. The helium recovery and purification device as claimed in claim 1, wherein the pressure transmitter (2) installed on the recovery gas tank (3) and the mass flow control meter (1) installed on the inlet pipeline cooperate to realize an interlocking function, so as to maintain the negative pressure environment of the recovery gas tank (3).
6. The helium recovery and purification device according to claim 1, wherein the gas purification columns (9) are internally filled with any one of molecular sieves, activated carbon or filtering mechanisms, and at least one set of gas redistribution devices is arranged in each set of gas purification columns (9).
7. The helium recovery and purification device as claimed in claim 1, wherein the control valve (7) is any one of a solenoid valve, a pneumatic valve and an electric valve.
8. A helium recovery and purification device as claimed in claim 1, wherein the off-gas outlet of said gas membrane separator (5) is fitted with one of a back pressure valve (6), a throttle valve or an electrically controlled proportional valve.
9. A method of recovery and purification using the helium recovery and purification apparatus of any one of claims 1 to 8, comprising the steps of: the used helium is metered by a mass flow controller I (1), recovered and enters a recovery gas tank (3), under the action of a recovery compression pump (4), the helium enters a gas membrane separator (5), the separated helium enters a gas purification tower (9) under the control of a control valve (7), and the purified helium is metered by a mass flow controller II (11) and enters helium using equipment.
CN202010516292.XA 2020-06-09 2020-06-09 Helium recovery and purification device and method Pending CN111573643A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
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Publication number Priority date Publication date Assignee Title
CN113247872A (en) * 2021-05-31 2021-08-13 安徽中科皖能科技有限公司 Recovery and purification device of low-concentration helium

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