CN115155246A - Low-concentration hydrogen adsorption purification method - Google Patents
Low-concentration hydrogen adsorption purification method Download PDFInfo
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- CN115155246A CN115155246A CN202210955401.7A CN202210955401A CN115155246A CN 115155246 A CN115155246 A CN 115155246A CN 202210955401 A CN202210955401 A CN 202210955401A CN 115155246 A CN115155246 A CN 115155246A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/02—Separation 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
- B01D53/04—Separation 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
- B01D53/047—Pressure swing adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/16—Hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/102—Nitrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/10—Single element gases other than halogens
- B01D2257/11—Noble gases
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7022—Aliphatic hydrocarbons
- B01D2257/7025—Methane
Abstract
The invention provides a low-concentration hydrogen adsorption purification method, and belongs to the field of gas separation. The invention adopts a basic purification system and a plurality of additional systems to combine, and directly adsorbs and separates the low-concentration hydrogen in the C-type mixed gas (especially natural gas) according to the requirement to obtain the hydrogen with different purities. The method is suitable for low-concentration hydrogen purification scenes, including but not limited to purification of industrial waste gas under low hydrogen concentration, purification of natural gas in-station, float glass manufacturing and the like.
Description
Technical Field
The invention belongs to the field of gas separation, relates to the field of direct hydrogen adsorption and purification, and particularly relates to a low-concentration hydrogen adsorption and purification method.
Background
According to incomplete statistics, the carbon emission of automobiles in 2018 in China is close to 20 hundred million tons, and how to reduce the carbon emission becomes a focus of increasing attention of people at present. As a substitute of the traditional automobile, the hydrogen fuel cell vehicle can really realize the aim of zero carbon emission and is the most effective way for solving the problem of carbon emission of automobile exhaust. Therefore, the purification technology and the transportation technology of hydrogen are the foundation for realizing the application of the hydrogen fuel cell vehicle.
PSA-H is mostly adopted in the current industrial purification method of fuel hydrogen 2 The precondition of this conventional method is that the hydrogen content in the feed gas should be higher than 50% and have a certain pressure. The transportation technique is divided into high-pressure gasBottle transportation, metal hydrogen storage transportation and pipeline transportation. Wherein, the transportation of the high-pressure gas cylinder is dangerous; the metal hydrogen storage transportation needs metal alloy as a carrier, and the transportation amount is extremely limited; pipeline transportation is a common method for gas transportation, but a large number of pipelines need to be laid, and the infrastructure investment is high.
At present, a certain amount of hydrogen is mostly mixed into a natural gas pipeline in pipeline transportation at home and abroad, the method has the advantages that only the existing natural gas pipeline is utilized, the investment cost of infrastructure in the hydrogen transportation process is greatly reduced, and the defects that the amount of the hydrogen mixed into the natural gas is limited, and the hydrogen concentration is very low and is generally not higher than 10 percent are overcome. By PSA-H 2 The power consumption is extremely high, and the purity of hydrogen extraction is difficult to reach more than 90%. The adsorption capacity of the existing adsorbent to methane is almost unchanged under high pressure, the pressure equalizing frequency of the PSA method is too many, the equipment is complex and the investment is high.
In the traditional method for purifying hydrogen, an adsorbent for adsorbing impurities in hydrogen is generally used, the hydrogen is used as a non-adsorption phase, and the direct purification of low-concentration hydrogen to more than 99 percent is difficult to realize. When the membrane separation method is adopted to purify the hydrogen, the purification can be realized only by a metal palladium membrane diffusion method. However, the palladium membrane has high production cost and low hydrogen permeation rate, and cannot be applied to large-scale industrialization.
Therefore, it is desirable to provide a new method for low-concentration hydrogen adsorption purification, which can realize high purity, high efficiency and high yield of hydrogen separation at a low cost.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a low-concentration hydrogen adsorption purification method, which aims to directly adsorb and separate low-concentration hydrogen in C-type mixed gas (especially natural gas) to obtain high-purity hydrogen.
The technical scheme provided by the invention is as follows:
a low-concentration hydrogen adsorption purification method is characterized in that a basic purification system and a plurality of additional systems are combined according to the hydrogen purification requirements of different raw material gases, wherein the basic purification system and the additional systems are composed of a plurality of adsorption towers which are connected in series, each adsorption tower in the basic purification system and the additional systems is filled with an adsorbent with hydrogen absorption capacity, the basic purification system and all the additional systems are connected in series, the raw material gas enters the basic purification system under certain pressure, each adsorption tower in the basic purification system is used for purifying hydrogen, impurity gas in the raw material gas is discharged from the adsorption towers, hydrogen obtained by the basic purification system is used as the raw material gas to enter the additional system which is connected in series with the basic purification system, each adsorption tower of the additional system is used for further purifying the hydrogen, meanwhile, the impurity gas is discharged from the adsorption towers, and the hydrogen purified by the additional systems is used as the raw material gas to enter another additional system which is connected in series with the additional systems until product gas is discharged from the endmost additional system.
The basic purification system meets the requirement that the purity of purified hydrogen is 80-99%, the number N of adsorption towers in the system is given by a formula (1), wherein P is adsorption pressure, K is pressure in each pressure equalizing process, the value range is 0.4-1 MPa, and the optimization range is 0.6-0.8 MPa;
the additional system consists of 2-4 adsorption towers connected in series. The filling amount M of the adsorbent in the single adsorption tower in the basic purification system and the additional system is calculated by the formula (2),
wherein t is the adsorption time, eta is the dynamic adsorption constant, F is the flow rate of the raw material gas,
and theta is the hydrogen percentage concentration, and theta is the static adsorption quantity of hydrogen.
Eta is 0.3-0.9.
The adsorption time t ranges from 60s to 1200s.
The adsorption pressure in the adsorption process of the adsorption tower is 0-20 MPa, and the desorption pressure is-90-0 MPa.
The adsorption temperature range in the adsorption process is 40-300 ℃, and the optimized temperature is 60-180 ℃.
The adsorbent comprises AB type, AB 2 Type AB 5 Type A 2 Form B, or A 2 B 7 The adsorbent is a type adsorbent, wherein A represents one or more elements of Mg, ti, zr, ce, la, V and the like; b represents one or more elements of Cr, mn, fe, ni, co, al, cu, zn, ga and the like. The adsorbent has an adsorption capacity of not less than 30ml/g and an optimized adsorption capacity of not less than 60ml/g under the change of working temperature (operating pressure).
The feed gas is formed by mixing hydrogen and C gas, the concentration of the hydrogen is 50% or less, and the C gas is N 2 ，Ar 2 ，CH 4 ，CO 2 A gas.
The number of said additional systems is 1-5.
And a compressor or a plurality of valves and an analysis instrument are arranged on a pipeline which is connected with the basic purification system and the additional system in series.
The invention has the following beneficial effects:
the invention can meet the requirements of hydrogen with different purities (2N-15N) by using the combination of a basic purification system and additional systems with different numbers: the basic purification system can meet the requirement that the purity of the hydrogen is 80-99 percent; the combination of the basic purification system and an additional system can meet the requirement that the purity of the hydrogen is 99-99.99 percent; the combination of the basic purification system and the two additional systems can meet the requirement that the purity of the hydrogen is 99.99-99.99999%; the combination of the basic purification system and the three additional systems can meet the requirement that the purity of the hydrogen is 99.99999% -99.99999999%; the combination of the basic purification system and the four additional systems can meet the requirement that the purity of the hydrogen is 99.99999999-99.99999999999%; the combination of the basic purification system and five additional systems can meet the requirement that the hydrogen purity is 99.99999999999% -99.9999999999999%. The method is suitable for low-concentration hydrogen purification scenes, including but not limited to purification of industrial waste gas under low hydrogen concentration, purification of natural gas in-station, float glass manufacturing and the like.
Drawings
FIG. 1 is a schematic view of a basic purification system in combination with an additional system of the present invention;
FIG. 2 is a schematic diagram of the structure of the adsorption columns in the basic purification system and the additional system in an embodiment of the present invention.
Detailed Description
The invention will be further described and illustrated with reference to specific embodiments without in any way limiting the scope of the invention.
Case one:
this requirement is met by using a basic purification system in combination with two additional systems, as shown in figure 1, depending on the desired product hydrogen concentration of 99.9999%.
The basic purification system and the additional system are connected in series, and the middle of the pipeline connected in series is provided with 2 compressors. The adsorbent is AB 5 Adsorbent LaNi 5 The raw material gas is 80% Ar 2 /20％H 2 The adsorption temperature of the mixed gas of (3) is 100 ℃. The adsorption pressure is 2MPa, the desorption pressure is-0.5 MPa, and the air inlet flow is 2000m 3 H is the ratio of the total weight of the catalyst to the total weight of the catalyst. The number N of the adsorption towers of the basic purification system is represented by the formula
Given, where P is the adsorption pressure, K is the pressure during each pressure equalization, N =2MPa/0.7MPa +1=4. The basic purification system comprises 4 adsorption columns as shown in fig. 2. Wherein: the adsorption towers A-D are connected in series, and a plurality of valves and analytical instruments are arranged on pipelines connected in series. Each additional system consists of 4 adsorption towers connected in series, the two additional systems respectively comprise adsorption towers E-H connected in series, adsorption towers I-L connected in series and 8 adsorption towers in total. Raw material gas enters into adsorption towers A-D in a basic purification system from an air inlet end of the basic purification system under certain pressure, each adsorption tower is used for purifying hydrogen, impurity gas in the raw material gas is discharged from the other ends of the adsorption towers A-D respectively, the hydrogen obtained from an exhaust end of the basic purification system is used as the raw material gas to enter into adsorption towers E-H of an additional system connected with the raw material gas in series, each adsorption tower of the additional system is used for further purifying the hydrogen, the impurity gas is discharged from the adsorption towers and purifiedThe purified hydrogen is fed again as a raw gas to the adsorption towers I to L of another additional system, each of which is used for further purifying hydrogen, impurity gas is discharged from the adsorption towers, and finally, the discharge end of the additional system discharges the purified hydrogen as a product gas.
As shown in FIG. 2, the pressure swing adsorption process for each adsorption column in the basic purification system and the additional system is as follows:
adsorption: the raw material gas enters the adsorption tower from one end of the adsorption tower under certain pressure, hydrogen is adsorbed by a special adsorbent, and argon is taken as adsorption tail gas and discharged from the other end of the adsorption tower;
pressure equalizing: the raw material gas stops entering the adsorption tower, and the argon gas with higher pressure in the adsorption tower is sequentially put into other low-pressure adsorption towers which have finished regeneration along the adsorption direction.
Placing in sequence: continuously discharging argon in the adsorption tower, and finishing the forward discharging process when the detector detects that the discharged gas contains hydrogen;
emptying: discharging residual hydrogen in the adsorption tower from the gas inlet end of the adsorption tower;
pressurizing: the raw material gas enters an adsorption tower, and the pressure is increased to the adsorption set pressure.
The filling amount M of the adsorbent in each adsorption tower in the basic purification system and the additional system is calculated by the formula (2),
wherein t is adsorption time (3 min), eta is dynamic adsorption constant (0.5), and F is raw material gas flow (2000 m) 3 /h)，
As a percentage concentration of hydrogen (20%), θ is the amount of hydrogen statically adsorbed (100 ml/g). The adsorbent loading of each adsorption column was 400kg, for a total of 12 adsorption columns, and the total loading was 4.8t.
Through experimental detection, the combination of the basic purification system and the two additional systems can meet the requirement that the purity of the hydrogen is 99.99-99.99999%.
Case two:
this requirement is met by a basic purification system in combination with three additional systems, depending on the requirement that the desired product hydrogen concentration be 99.999999%. The adsorbent is A 2 Adsorbent type B Mg 2 Ni, raw material gas 90% by weight CH 4 /10％H 2 The adsorption temperature of the mixed gas of (3) is 60 ℃. The adsorption pressure is 4MPa, the desorption pressure is-1 MPa, and the air inlet flow is 600m 3 H is the ratio of the total weight of the catalyst to the total weight of the catalyst. The number of the adsorption towers in the basic purification system is 6 (N =4MPa/0.8MPa + 1), the number of the adsorption towers in each additional system is 4, and the total number of the adsorption towers in the basic system and the additional system is 18. The packing amount of the adsorbent in each adsorption tower was 125kg as calculated from the formula (2), wherein t is the adsorption time (5 min), η is the dynamic adsorption constant (0.5), and F is the feed gas flow rate (600 m) 3 /h)，
As a percentage concentration of hydrogen (10%), θ is the amount of hydrogen statically adsorbed (80 ml/g). Raw material gas enters adsorption towers in a basic purification system from a gas inlet end of the basic purification system under a certain pressure, each adsorption tower is used for purifying hydrogen, impurity gas in the raw material gas is discharged from the other end of each adsorption tower respectively, the hydrogen obtained in the basic purification system is used as the raw material gas and enters a first additional system, the hydrogen obtained by the first additional system is used as the raw material gas and enters a second additional system connected with the first additional system in series, the hydrogen obtained by the second additional system is used as the raw material gas and enters a third additional system connected with the second additional system in series, each adsorption tower in the additional system is used for further purifying the hydrogen, the impurity gas is discharged from the adsorption towers, and finally the purified hydrogen discharged by the third additional system is used as product gas.
The pressure swing adsorption process for each adsorption column in the basic purification system and the additional system is as follows:
adsorption: the raw material gas enters the adsorption tower from one end of the adsorption tower under certain pressure, hydrogen is adsorbed by a special adsorbent, and methane is taken as adsorption tail gas and discharged from the other end of the adsorption tower;
pressure equalizing: stopping the raw gas from entering the adsorption tower, and sequentially placing the high-pressure methane in the adsorption tower into other low-pressure adsorption towers which are subjected to regeneration along the adsorption direction;
placing in sequence: continuously discharging methane in the adsorption tower, and finishing the forward discharging process when the detector detects that the discharged gas contains hydrogen;
emptying: discharging residual hydrogen in the adsorption tower from the gas inlet end of the adsorption tower;
pressurizing: the raw material gas enters an adsorption tower, and the pressure is increased to the adsorption set pressure.
Through experimental detection, the combination of the basic purification system and the five additional systems can meet the requirement that the purity of the hydrogen is 99.99999% -99.99999999%.
The low-concentration hydrogen adsorption purification method provided by the invention can realize purification and separation of low-concentration hydrogen in the mixed gas of hydrogen and C-type gas. Different combinations of basic purification systems and additional systems can be used to obtain hydrogen of different purities, for example: the fuel hydrogen may be recommended to use the basic purification system in combination with one additional system, and the high purity hydrogen may be recommended to use the basic purification system in combination with two or three additional systems; ultra-high purity hydrogen may be recommended for the basic purification system in combination with four or five additional systems.
It is noted that the disclosed embodiments are intended to aid in further understanding of the invention, but those skilled in the art will appreciate that: various substitutions and modifications are possible without departing from the spirit and scope of the invention and appended claims. Therefore, the invention should not be limited by the disclosure of the embodiments, but should be defined by the scope of the appended claims.
Claims (10)
1. A low-concentration hydrogen adsorption purification method is characterized in that a basic purification system and a plurality of additional systems are combined according to the hydrogen purification requirements of different raw material gases, wherein the basic purification system and the additional systems are composed of a plurality of adsorption towers which are connected in series, an adsorbent with hydrogen absorption capacity is arranged in each adsorption tower of the basic purification system and the additional systems, the basic purification system and all the additional systems are connected in series, the raw material gases enter the basic purification system under certain pressure, each adsorption tower in the basic purification system is used for purifying hydrogen, impurity gases in the raw material gases are discharged from the adsorption towers, hydrogen obtained by the basic purification system enters the additional system which is connected in series with the raw material gases, each adsorption tower of the additional systems is used for further purifying the hydrogen, meanwhile, the impurity gases are discharged from the adsorption towers, and the hydrogen purified by the additional systems enters another additional system which is connected in series with the raw material gases until product gases are discharged from the endmost additional system.
2. The method for purifying by adsorption of low concentration hydrogen according to claim 1, wherein the purity of hydrogen obtained by the basic purification system is 80% to 99%, the number N of adsorption columns in the system is given by the following formula,
wherein P is the adsorption pressure of the adsorption tower, K is the pressure of the adsorption tower in the pressure equalizing process each time, and the value range of K is 0.4-1 MPa.
3. The adsorptive purification process for low concentration hydrogen gas according to claim 1, wherein said additional system comprises from 2 to 4 adsorption columns connected in series.
4. The method for adsorptive purification of low concentration hydrogen according to claim 2, wherein the loading M of adsorbent in each of the adsorption columns in the basic purification system and the additional system is calculated by the following formula,
wherein t is the adsorption time of the adsorption tower, eta is the dynamic adsorption constant, F is the flow rate of the raw material gas,
is the percentage concentration of the hydrogen gas,θ is the amount of hydrogen gas adsorbed statically.
5. The method for adsorbing and purifying low-concentration hydrogen according to claim 3, wherein η is in a range of 0.3 to 0.9, and the adsorption time t is in a range of 60s to 1200s.
6. The method for adsorbing and purifying low-concentration hydrogen according to claim 1, wherein the adsorption pressure in the adsorption process of the adsorption tower is in the range of 0 to 20MPa, the desorption pressure is in the range of-90 to 0MPa, and the adsorption temperature in the adsorption process is in the range of 40 to 300 ℃.
7. The low concentration hydrogen adsorption purification system of claim 1, wherein the number of additional systems is 1 to 5.
8. The system for adsorptive purification of low concentration hydrogen according to claim 1, wherein said basic purification system and said additional system are connected in series by a pipeline having a compressor or a plurality of valves and an analytical instrument.
9. The method of claim 1, wherein the adsorbent comprises AB, AB type 2 Type AB 5 Type A 2 Form B, or A 2 B 7 The adsorbent is a type adsorbent, wherein A represents one or more elements of Mg, ti, zr, ce, la, V and the like; b represents one or more elements of Cr, mn, fe, ni, co, al, cu, zn, ga and the like.
10. The method for adsorptive purification of low concentration hydrogen according to claim 1, wherein said feed gas is a mixture of hydrogen and a C-type gas, wherein the concentration of hydrogen is 50% or less, and said C-type gas is N 2 ，Ar 2 ，CH 4 ，CO 2 A gas.
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