CN112591710A - High-purity fuel hydrogen preparation and conveying system and control method thereof - Google Patents
High-purity fuel hydrogen preparation and conveying system and control method thereof Download PDFInfo
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- C01B3/501—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
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Abstract
The invention relates to a method and a system for preparing and conveying high-purity fuel hydrogen. The hydrogen-containing tail gas sequentially passes through a preparation and conveying system consisting of the gas phase purification device, the pressure swing adsorption device, the pipeline conveying device and the membrane separation device, the hydrogen-containing tail gas enters from one end of the gas phase purification device, enters the pressure swing adsorption device after impurity removal through the gas phase purification device, enters the pipeline conveying device after purification through the pressure swing adsorption device and then is conveyed to a user side, an outlet of the pipeline conveying device is connected with the membrane separation device, and fuel hydrogen is output after secondary purification is carried out by the membrane separation device. The system can obviously prolong the service life of the functional membrane, solve the problems of hydrogen transportation and storage and improve the economic benefit.
Description
Technical Field
The invention belongs to the technical field of high-purity hydrogen preparation and delivery, and particularly relates to a high-purity fuel hydrogen preparation and delivery system and a control method thereof, wherein hydrogen is derived from a byproduct hydrogen-containing tail gas of a chemical plant.
Background
Automobiles are one of the main causes of pollution caused by energy consumption, and therefore automobile companies in various countries are working on improving the emission and fuel usage of automobiles. In view of the current development, the pem fuel cell technology can effectively achieve the effect sought by the automobile companies, is a future development trend of electric vehicles recognized in the industry, and is expected to become a third-generation brand new power system after internal combustion engines and steam gas engines. In recent years, hydrogen fuel cell vehicles have been introduced by various automobile manufacturers worldwide.
The hydrogen is used as the necessary fuel of the fuel cell, and the preparation technology, the storage and transportation technology and the like determine whether the hydrogen fuel cell can be obtained conveniently, quickly and at low cost, so that the aim of mass production is fulfilled. The main hydrogen production technology and the hydrogen transportation mode at the present stage are as follows: and transporting the chlor-alkali by-product hydrogen + hydrogen by trailer. The chlorine-alkali secondary gas is used as hydrogen source, and the conventional separation process adopts one of a pressure swing adsorption device or a membrane separation device to separate the secondary gas so as to obtain high-purity hydrogen. However, in the process, the byproduct gas is not pretreated, particularly the content of carbon oxide is further reduced, so that carbon dioxide corrosion occurs, the service life of the separation membrane is reduced, and the pressure swing adsorption device is only adopted, so that the defects that the higher the purity of the hydrogen is, the more equipment is needed are overcome, and the membrane separation device is only adopted, so that the defect of low separation efficiency is also overcome. Meanwhile, the transportation of the gas hydrogen trailer has the defects of high transportation cost, high danger and the like. When the high-purity hydrogen is directly transported by a pipeline, hydrogen embrittlement is easy to occur, so that safety accidents occur, and meanwhile, the purity of the hydrogen product can be reduced by dissolving trace impurities in the transportation process, so that the use of the fuel cell is influenced. In order to overcome the above problems and stably obtain high-quality fuel hydrogen, it is necessary to develop and design a production and transportation combined method having superior economy and safety based on the optimal economic consideration of production cost and transportation cost.
Therefore, in order to achieve the above objects, further reduce the content of impurities in the gas source, increase the service life of the functional membrane, solve the problems of safety and easy pollution in transportation, and realize continuous supply of high-purity fuel hydrogen, the invention provides a method and a system for preparing and conveying high-purity fuel hydrogen. The hydrogen source is pretreated by designing the gas phase purification device, and the pressure swing adsorption device, the pipeline conveying device and the membrane separation device are reasonably combined in process design, so that the problems of hydrogen brittleness, pollution and the like in pipeline transportation are solved, and finally the high-purity fuel hydrogen is stably obtained.
Disclosure of Invention
The invention aims to provide a method and a system for preparing and conveying high-purity fuel hydrogen, which take hydrogen-containing tail gas as a raw material, solve the problems of short service life of a functional membrane, hydrogen brittleness of equipment and easy pollution of fuel hydrogen and realize continuous supply of high-purity fuel hydrogen.
A high-purity fuel hydrogen preparation and conveying system comprises a gas phase purification device, a pressure swing adsorption device, a pipeline conveying decoration and a membrane separation device; the outlet of the gas phase purification device is connected with the pressure swing adsorption device, the outlet of the pressure swing adsorption device is connected with the pipeline conveying device, and the outlet of the pipeline conveying device is connected with the membrane separation device;
hydrogen-containing tail gas enters from one end of the gas phase purification device, enters the pressure swing adsorption device after impurity removal of the gas phase purification device, enters the pipeline conveying device after purification of the pressure swing adsorption device and then is conveyed to a user side, an outlet of the pipeline conveying device is connected with the membrane separation device, and after secondary purification is carried out by utilizing the membrane device, a fuel hydrogen product is output.
Furthermore, the gas phase purification device comprises a front buffer tank, a compressor, a rear buffer tank, a freeze dryer, a front precision filter, a gas phase purification adsorption column and a rear precision filter.
Furthermore, the material of the adsorbent is one or a mixture of guanidinium ionic liquid, nitrilamine ionic liquid and quaternary phosphonium ionic liquid, such as: 1,1,3, 3-tetramethylguanidine-5-cyanotetrazole seed liquid, methoxytriethoxyethylpyridine tricyanamide seed liquid, triethylmonomethyl quaternary phosphonium imidazole seed liquid, and the like.
Furthermore, the operation pressure is-0.05-5.0 MPa, and the temperature is 0-50 ℃.
Further, the functional membrane is a cross-linked hollow fiber anion exchange membrane loaded with metallic palladium.
Furthermore, the operating pressure of the freeze dryer is 0.1-1.5 MPa, and the temperature is 0-20 ℃.
Furthermore, the pressure of the permeation side of the membrane separator is-0.09-0.2 MPa.
Furthermore, the pressure of the retentate side of the membrane separator is 0.1-1.5 MPa.
Still further, a method of controlling a high purity fuel hydrogen production and delivery system, comprising:
step 1: hydrogen-containing tail gas firstly enters a gas phase purification device; after being buffered by a front buffer tank of the gas phase purification device, the gas phase purification device enters a compressor for pressurization and then enters a rear buffer tank for buffering; then introducing the mixture into a freeze dryer for quick freezing to remove liquid components; then removing trace solid particle impurities through a preposed precision filter; introducing the filtered hydrogen-containing gas into a gas phase purification adsorption column, filtering the purified gas again by a post-positioned precision filter, and supplying the gas to a pressure swing adsorption device;
step 2: the inlet of the pressure swing adsorption device is directly connected with the outlet of the gas phase purification device, and the outlet of the pressure swing adsorption device obtains hydrogen with the purity of 90-99 percent, and the purity of the hydrogen can be adjusted according to the actual working condition;
step 3: the outlet of the pressure swing adsorption device is directly connected with the existing pipeline conveying device and conveyed to a user end;
step 4: the hydrogen sent to the user end through the pipeline conveying device is directly connected with the inlet of the membrane separation device and enters the membrane separation device for secondary purification.
Furthermore, the pretreated feed gas enters a membrane separator of a core for hydrogen repurification, the separation membrane is provided with a permeation side and a retentate side, the permeation side is provided with a vacuum pump, a pressure regulating valve and a circulating pipeline, the hydrogen permeating into the permeation side from the functional membrane is pumped out and obtained, and the hydrogen is used as a fuel hydrogen product and output to an outlet buffer tank, and the purity is not lower than 99.999%.
The invention has the advantages that:
1. by adopting the gas phase purification device, the raw material gas is pretreated, and the service life of the functional membrane is prolonged.
2. The gas phase purification device adopts the developed ionic liquid adsorbent, can deeply adsorb and remove carbon oxides mainly containing carbon dioxide, and can reduce the concentration of the carbon dioxide to be less than 10 ppm.
3. By adopting the combined process of the pressure swing adsorption device, the pipeline conveying device and the membrane separation device, the advantages of large treatment capacity of the pressure swing adsorption technology and high purity of the membrane separation technology can be fully exerted, the high energy consumption and the operation cost brought by repeated separation for many times are solved, and meanwhile, the phenomenon that the pipeline is easy to become hydrogen brittle when high-purity hydrogen is conveyed can be avoided.
Drawings
FIG. 1: a process flow chart of preparing and conveying high-purity fuel hydrogen;
FIG. 2: a gas phase purification device process flow diagram;
FIG. 3: a process flow diagram of a functional membrane separation device;
description of reference numerals:
i-gas phase purification device (front buffer tank (I1), compressor (I2), back buffer tank (I3), freeze dryer (I4), front precision filter (I5), gas phase purification adsorption column (I6A/B), back precision filter (I7));
II, a pressure swing adsorption device;
III-a pipe conveying device;
IV-membrane separation device (buffer tank (IV1), lyophilizer (IV2), pre-precision filter (IV3), membrane separator (IV4), vacuum pump (IV5), pressure regulating valve (IV6) and outlet buffer tank (IV 7)).
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
The invention relates to a system for preparing and delivering high-purity fuel hydrogen, which comprises: a gas phase purification device (I), a pressure swing adsorption device (II), a pipeline conveying device (III) and a membrane separation device (IV). The outlet of the gas phase purification device (I) is connected with the pressure swing adsorption device (II), the outlet of the pressure swing adsorption device (II) is connected with the pipeline conveying device (III), and the outlet of the pipeline conveying device (III) is connected with the membrane separation device (IV).
And an ionic liquid adsorbent is filled in a gas phase purification adsorption column (I5A/B) in the gas phase purification device (I) and is used for pretreating hydrogen-containing tail gas.
The membrane separator (IV4) in the membrane separation device (IV) adopts a cross-linked hollow fiber anion exchange membrane loaded with metal palladium for deep purification of hydrogen.
The operation method for preparing and conveying the high-purity fuel hydrogen comprises the following steps:
the hydrogen-containing tail gas is firstly introduced into a front buffer tank (I1) of a gas phase purification device (I) for buffering, then is sucked into a compressor (I2) for pressurization and then enters a rear buffer tank (I3) for buffering. The compressed gas phase is introduced into a freeze dryer (I4) for quick freezing to remove liquid components, and then a pre-precision filter (I5) is used for removing trace solid particle impurities. The filtered hydrogen-containing gas is introduced into a gas phase purification adsorption column (I6), and the purified gas is filtered again by a post-precise filter (I7) and then is supplied to a pressure swing adsorption device (II).
The purified hydrogen-containing tail gas enters a pressure swing adsorption device (II) for hydrogen purification.
The outlet of the pressure swing adsorption device (II) is directly connected with the existing pipeline conveying device (III) to convey the primarily purified hydrogen to the user end.
The hydrogen sent to the user end through the pipeline conveying device (III) is directly connected with the inlet of the membrane separation device (IV) and enters the membrane separation device for secondary purification. The gas phase at the inlet is buffered by a buffer tank (IV1) and then enters a freeze dryer (IV2) to remove easily condensable components through low-temperature condensation; then leading the mixture to a preposed precision filter (IV3) to remove solid impurities so as to prevent the separation membrane from being blocked; the pretreated feed gas enters a membrane separator (IV4) in the core for hydrogen repurification. The separation membrane is provided with a permeate side and a retentate side. The permeation side is provided with a vacuum pump (IV5), a pressure regulating valve (IV6) and a circulating pipeline, and the pressure difference formed between the permeation side and the inlet side is permeation by hydrogen. The hydrogen permeating from the functional membrane into the permeation side is pumped out to obtain a fuel hydrogen product, and the gas discharged from the permeation side of the membrane can be used as a common fuel.
Example 1
Hydrogen-containing tail gas which is a byproduct of a chlor-alkali enterprise and enters a designed high-purity fuel hydrogen preparation and conveying system at the flow rate of 50ml/min, firstly enters a pressure swing adsorption device (II) for primary purification of hydrogen after being purified by a gas phase purification device to obtain the hydrogen with the purity of 98%, and then is conveyed to a membrane separation device at a user end through a pipeline conveying device for secondary purification. The adsorbent filled in the gas phase purification adsorption column is 1,1,3, 3-tetramethylguanidine-5-cyanotetrazole liquid, the operating pressure is 3.0MPa, and the operating temperature is 25 ℃. The operating pressure of the freeze dryer is 3.2MPa, and the operating temperature is 25 ℃.
Used in the membrane separation device was a metal palladium-supported cross-linked hollow fiber anion exchange membrane in which the metal palladium loading was 3%. The operating pressure of the freeze dryer is 1.2MPa, and the operating temperature is 2 ℃. The pressure of the permeation side of the membrane separator is-0.05 MPa, and the pressure of the retentate side is 1.15 MPa.
After the system continuously and stably operates for 120min, samples at the inlet and the outlet of the system are simultaneously taken for analysis, and the analysis results are shown in table 1.
[ Table 1]
| Inlet port | An outlet | |
| Hydrogen content | 99％ | ＞99.999％ |
| CO | 5ppm | 2.6ppm |
| CO2 | 52ppm | 9ppm |
| H2O | 6000ppm | 200ppm |
After the hydrogen-containing tail gas is purified and separated by a designed high-purity fuel hydrogen preparation and conveying system, the concentration of carbon oxygen compounds in the obtained fuel hydrogen product is obviously reduced, particularly the concentration of carbon dioxide is reduced to 9ppm, and the purity of the fuel hydrogen product is also higher than 99.999%.
Example 2
The same hydrogen-containing tail gas in example 1 was fed into a pressure swing adsorption apparatus (II) at a flow rate of 50ml/min to primarily purify hydrogen, to obtain 98% pure hydrogen, which was then sent to a membrane separation apparatus at the user end via a pipeline transport apparatus to be purified again. In comparison with example 1, a gas phase purification device was absent.
Used in the membrane separation device was a metal palladium-supported cross-linked hollow fiber anion exchange membrane in which the metal palladium loading was 3%. The operating pressure of the freeze dryer is 1.2MPa, and the operating temperature is 2 ℃. The pressure of the permeation side of the membrane separator is-0.05 MPa, and the pressure of the retentate side is 1.15 MPa.
After the system continuously and stably runs for 120min, samples at the inlet and the outlet of the system are simultaneously taken for analysis, and the analysis results are shown in table 2.
[ Table 2]
| Inlet port | An outlet | |
| Hydrogen content | 99％ | ＞99.999％ |
| CO | 5ppm | 4.5ppm |
| CO2 | 52ppm | 44ppm |
| H2O | 6000ppm | 232ppm |
The hydrogen product purity of the fuel obtained is higher than 99.999%, but the carbon oxide concentration is almost unchanged compared with the feed in the absence of a gas phase purification device.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A high purity fuel hydrogen production and delivery system, characterized by: the system comprises a gas phase purification device, a pressure swing adsorption device, a pipeline conveying decoration and membrane separation device; the outlet of the gas phase purification device is connected with the pressure swing adsorption device, the outlet of the pressure swing adsorption device is connected with the pipeline conveying device, and the outlet of the pipeline conveying device is connected with the membrane separation device;
hydrogen-containing tail gas enters from one end of the gas phase purification device, enters the pressure swing adsorption device after impurity removal of the gas phase purification device, enters the pipeline conveying device after purification of the pressure swing adsorption device and then is conveyed to a user side, an outlet of the pipeline conveying device is connected with the membrane separation device, and fuel hydrogen is output after secondary purification is carried out by the membrane separation device.
2. A high purity fuel hydrogen production and delivery system as defined in claim 1, wherein said gas phase purification apparatus comprises a front buffer tank, a compressor, a rear buffer tank, a freeze dryer, a front precision filter, a gas phase purification adsorption column, a rear precision filter.
3. A high purity fuel hydrogen production and delivery system as claimed in claim 1, wherein the adsorbent material is selected from one or a mixture of guanidinium ionic liquids, nitrilamine ionic liquids, quaternary phosphonium ionic liquids.
4. A high purity fuel hydrogen production and delivery system as claimed in claim 1, wherein the operating pressure is-0.05 to 5.0MPa and the temperature is 0 to 50 ℃.
5. A high purity fuel hydrogen production and delivery system as in claim 1 wherein the functional membrane is a metal palladium supported cross-linked hollow fiber anion exchange membrane.
6. The system for preparing and delivering high purity fuel hydrogen as claimed in claim 1, wherein the freeze dryer is operated at a pressure of 0.1-1.5 MPa and a temperature of 0-20 ℃.
7. The high purity fuel hydrogen production and delivery system of claim 1, wherein the membrane separator permeate side pressure is-0.09 to 0.2 MPa.
8. The high purity fuel hydrogen production and delivery system of claim 1, wherein the membrane separator retentate side pressure is 0.1 to 1.5 MPa.
9. The method of controlling a high purity fuel hydrogen production and delivery system of claim 1,
step 1: hydrogen-containing tail gas firstly enters a gas phase purification device; after being buffered by a front buffer tank of the gas phase purification device, the gas phase purification device enters a compressor for pressurization and then enters a rear buffer tank for buffering; then introducing the mixture into a freeze dryer for quick freezing to remove liquid components; then removing trace solid particle impurities through a preposed precision filter; introducing the filtered hydrogen-containing gas into a gas phase purification adsorption column, filtering the purified gas again by a post-positioned precision filter, and supplying the gas to a pressure swing adsorption device;
step 2: the inlet of the pressure swing adsorption device is directly connected with the outlet of the gas phase purification device, and the outlet of the pressure swing adsorption device obtains hydrogen with the purity of 90-99 percent, and the purity of the hydrogen can be adjusted according to the actual working condition;
step 3: the outlet of the pressure swing adsorption device is directly connected with the existing pipeline conveying device and conveyed to a user end;
step 4: the hydrogen sent to the user end through the pipeline conveying device is directly connected with the inlet of the membrane separation device and enters the membrane separation device for secondary purification.
10. The method of claim 9 wherein the pretreated feed gas is fed to a membrane separator in the core for hydrogen repurification, the separation membrane has a permeate side and a retentate side, the permeate side is provided with a vacuum pump, a pressure regulating valve and a circulation line, and the hydrogen permeating from the functional membrane into the permeate side is pumped out and obtained as a fuel hydrogen product to be output to an outlet buffer tank, wherein the purity of the hydrogen product is not less than 99.999%.
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