CN111924803A - Hydrogen purification process technology - Google Patents
Hydrogen purification process technology Download PDFInfo
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- CN111924803A CN111924803A CN202010715872.1A CN202010715872A CN111924803A CN 111924803 A CN111924803 A CN 111924803A CN 202010715872 A CN202010715872 A CN 202010715872A CN 111924803 A CN111924803 A CN 111924803A
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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
- 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
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0415—Purification by absorption in 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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/042—Purification by adsorption on 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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/0475—Composition of the impurity the impurity being carbon dioxide
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/048—Composition of the impurity the impurity being an organic compound
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
- C01B2203/0465—Composition of the impurity
- C01B2203/0495—Composition of the impurity the impurity being water
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Abstract
The invention discloses a hydrogen purification process technology, wherein the total reaction mixed gas comprises CH4, H2O, C02 and H2, a primary cooler removes water vapor, a methane absorption tank removes methane by melting methane into carbon tetrachloride solvent, a carbon dioxide reaction kettle removes carbon dioxide by CaCO3+ H2O + CO2= Ca (HCO3)2, a secondary cooler removes a very small amount of water vapor in the air, the whole process is carried out in vacuum, and hydrogen with the purity of 99.5-99.9% is further obtained.
Description
Technical Field
The invention relates to the technical field of hydrogen purification, in particular to a hydrogen purification process technology.
Background
Hydrogen (Hydrogen) is the lightest gas known in the world. Its density is very small, 1/14 for air alone, i.e., 0.0899g/L for hydrogen at 0 ℃ under standard atmospheric pressure. Hydrogen (H2) was synthesized artificially at the earliest and early 16 th century, when metals were placed in strong acids. 1766 + 1781, henli carvedilol discovered that hydrogen is another gas than previously found, and produced water when burned, a property that also determines the name "hydrogen" for the term "water-producing substance". At normal temperature and pressure, hydrogen is a gas which is extremely easy to burn, colorless, transparent, odorless and tasteless.
With the development of society, the demand of hydrogen is increasing day by day, so hydrogen purification treatment needs to be carried out continuously, and the prior purification process equipment of hydrogen is complex, gas mixing reaction in a plurality of purification processes has more removal side reactions, and the purification equipment of hydrogen is expensive and is not convenient for being popularized vigorously corresponding to small and medium-sized factories.
Therefore, we propose a hydrogen purification process technology.
Disclosure of Invention
The invention aims to provide a purification process technology of hydrogen, mixed gases obtained through total reaction are CH4, H2O, C02 and H2, a primary cooler removes water vapor, a methane absorption tank removes methane by melting the methane into a carbon tetrachloride solvent, a carbon dioxide reaction kettle removes carbon dioxide by CaCO3+ H2O + CO2= Ca (HCO3)2, a secondary cooler removes a very small amount of water vapor in the air, and the whole process is carried out in vacuum, so that the hydrogen with the purity of 99.5-99.9% is obtained, and the problems brought forward in the background are solved.
In order to achieve the purpose, the invention provides the following technical scheme: a hydrogen purification process technology comprises the following steps:
s1: general reaction
Respectively and simultaneously introducing natural gas and water vapor into a sealed main reaction kettle, setting the internal temperature to be 600-plus-800 ℃ and the pressure to be 0.1013Pan, wherein the reaction is an intermittent operation reaction, and the water vapor is subjected to high-temperature treatment at 600-plus-500 ℃ before introduction;
s2: first order water vapor removal
Introducing a primary mixed gas obtained by the primary S1 total reaction kettle reaction into an S-shaped cooling pipeline, conveying the primary mixed gas into a primary cooler, cooling the primary mixed gas to 23-28 ℃, and removing water vapor in the primary mixed gas; s3: methane removal
Introducing the secondary mixed gas at normal temperature into a methane absorption tank by using a U-shaped pipe, wherein one end of the U-shaped pipe is inserted into the bottom of the methane absorption tank, and removing methane in the secondary mixed gas;
s4: carbon dioxide removal
Introducing the three-stage mixed gas into a carbon dioxide reaction kettle by using a U-shaped pipe, wherein one end of the U-shaped pipe is inserted into the bottom of the carbon dioxide reaction kettle, and removing carbon dioxide in the three-stage mixed gas;
s5: two stage water vapor removal
And repeating S2, introducing the third-stage mixed gas into the fourth-stage mixed gas in the second-stage cooler, cooling to 1-5 ℃, discharging high-purity hydrogen, and introducing into a gas collection tank.
Further, the chemical equation of the total reaction kettle is CH4+ H2O = CO + H2, CO + H20= C02+3H2, the catalyst is nickel, the primary mixed gas is CH4, H2O, C02 and H2, and the concentration of hydrogen discharged from the device is 70-75%.
Further, the water vapor in the S1 is excessively filled and is 1.3-1.8 times of the natural gas amount, the reaction amount ratio of the initial natural gas to the water vapor is 1:1 for reaction, and the redundant natural gas is filled in by a subsequent filling mode.
Further, the primary mixed gas is CH4, H2 and C02 and a large amount of water vapor, the secondary mixed gas is CH4, C02 and H2 and a small amount of water vapor, the tertiary mixed gas is C02 and H2 and a small amount of water vapor, the quaternary mixed gas is H2 and a very small amount of water vapor, and the concentration of H2 is 99.5-99.9%.
Further, 2/3 carbon tetrachloride solvent is filled in the methane absorption tank.
Further, the carbon dioxide reaction kettle is filled with 2/3 limestone solution, and the reaction equation is CaCO3+ H2O + CO2= Ca (HCO3) 2.
Further, before each hydrogen purification, vacuum-pumping treatment needs to be performed in the pipeline and the equipment.
Compared with the prior art, the method has the advantages that the total reaction mixed gas is CH4, H2O, C02 and H2, the first-stage cooler removes water vapor, the methane absorption tank removes methane by melting the methane into carbon tetrachloride solvent, the carbon dioxide reaction kettle removes carbon dioxide by CaCO3+ H2O + CO2= Ca (HCO3)2, the second-stage cooler removes a very small amount of water vapor in the air, the whole process is carried out in vacuum, hydrogen with the purity of 99.5-99.9% is further obtained, the purification process is high in pertinence and is removed one by one, the purification equipment is simplified, the equipment cost is low, the cost of purified hydrogen for small and medium enterprises is low, and the method is convenient to popularize.
Drawings
FIG. 1 is a flow diagram of the purification process of the present invention;
FIG. 2 is a schematic view of the purification process apparatus of the present invention.
In the figure: 1. a total reaction kettle; 2. a primary cooler; 3. a methane absorption tank; 4. a carbon dioxide reaction kettle; 5. a secondary cooler; 6. a gas collection tank.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, a hydrogen purification process includes the following steps:
the first embodiment is as follows:
before each hydrogen purification, the inside of pipelines and equipment needs to be vacuumized, the influence of gases such as oxygen, hydrogen and the like in the air on the purification process is reduced, natural gas and water vapor are respectively and simultaneously introduced into a sealed total reaction kettle 1, the internal temperature is set to be 600-800 ℃, the pressure is 0.1013Pan, the reaction is an intermittent operation reaction, so that a large amount of natural gas and water vapor cannot be mixed when reaction mixed gas is extracted, the water vapor is subjected to high-temperature treatment at the temperature of 500-600 ℃ before introduction, the chemical equation of the total reaction kettle 1 is CH4+ H2O = CO + H2, CO + H20= C02+3H2, the catalyst is nickel, the water vapor in S1 is excessively charged and is 1.3-1.8 times of the natural gas amount, the reaction amount ratio of the initial natural gas to the water vapor is 1:1, and the redundant natural gas is introduced in a subsequent charging mode, so that the water vapor is excessively charged, can fully react with natural gas, reduce the amount of methane in the primary mixed gas to the maximum extent, react CO generated by the reaction to form C02, and further reduce the amount of the mixed gas, wherein the primary mixed gas is CH4, H2O, C02 and H2, and the concentration of hydrogen discharged from the device is 70-75%.
Example two: the mixed gas in the first embodiment comprises CH4, H2O, C02 and H2, and further purification is needed;
the primary mixed gas of the primary S1 total reaction kettle 1 is conveyed to the primary cooler 2 through the S-shaped cooling pipeline, the primary mixed gas can be subjected to preliminary cooling treatment by the S-shaped cooling pipeline, when the primary mixed gas is conveyed to the primary cooler 2, the cooling speed is higher, the temperature of the primary mixed gas is cooled to 23-28 ℃, water vapor in the primary mixed gas is removed, and the secondary mixed gas is CH4, C02, H2 and a small amount of water vapor. Example three: the mixed gas in the second embodiment comprises CH4, C02, H2 and a small amount of water vapor, and further purification is needed;
the second grade mist with the normal atmospheric temperature utilizes the U-shaped pipe to let in methane absorption tank 3, and the one end of U-shaped pipe is for inserting 3 bottoms of methane absorption tank, can prevent that the liquid from flowing backward, can make mist and solvent or liquid intensive mixing again, and the inside carbon tetrachloride solvent that is filled with 2/3 of methane absorption tank 3, when methane emerges from the carbon tetrachloride solvent, can melt in the carbon tetrachloride solvent, and then get rid of methane, and tertiary mist is C02, H2 and a small amount of vapor.
Example four: the mixed gas in the third example comprises C02, H2 and a small amount of water vapor, and further purification is needed:
the tertiary mixed gas is introduced into a carbon dioxide reaction kettle 4 by using a U-shaped pipe, one end of the U-shaped pipe is inserted into the bottom of a methane absorption tank 3, the carbon dioxide reaction kettle 4 is filled with 2/3 limestone solution, and the reaction equation is CaCO3+ H2O + CO2= Ca (HCO3)2, when the tertiary mixed gas emerges from the bottom of the limestone solution, the CO2 in the tertiary mixed gas can be completely removed through the reaction of the reaction equation CaCO3+ H2O + CO2= Ca (HCO3) 2.
Example five: the mixed gas in example four, comprising H2 and a small amount of water vapor, required further purification:
and repeating S2, introducing the third-stage mixed gas into a second-stage cooler 5, discharging a fourth-stage mixed gas, cooling to the temperature of 1-5 ℃, further condensing a small amount of water vapor in the air, further improving the purity of the hydrogen, finally discharging high-purity hydrogen, and introducing into a gas collection tank 6, wherein the fourth-stage mixed gas is H2 and a very small amount of water vapor, and the concentration of H2 is 99.5-99.9%.
In summary, the following steps: the invention provides a hydrogen purification process technology, which comprises the steps of obtaining mixed gases of CH4, H2O, C02 and H2 through total reaction, removing water vapor through a primary cooler 2, removing methane through a methane absorption tank 3 by melting methane into a carbon tetrachloride solvent, removing carbon dioxide through CaCO3+ H2O + CO2= Ca (HCO3)2 in a carbon dioxide reaction 4 kettle, removing a very small amount of water vapor in the air through a secondary cooler 5, and performing the whole process in vacuum to obtain hydrogen with the purity of 99.5-99.9%.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The hydrogen purification process technology is characterized by comprising the following technical steps:
s1: general reaction
Respectively and simultaneously introducing natural gas and water vapor into a sealed main reaction kettle (1), setting the internal temperature to be 600-plus-800 ℃ and the pressure to be 0.1013Pan, wherein the reaction is an intermittent operation reaction, and the water vapor is subjected to high-temperature treatment at the temperature of 500-plus-600 ℃ before introduction;
s2: first order water vapor removal
Introducing a primary mixed gas reacted in the primary S1 total reaction kettle (1) into an S-shaped cooling pipeline and conveying the primary mixed gas into a primary cooler (2), cooling the primary mixed gas to 23-28 ℃, and removing water vapor in the primary mixed gas; s3: methane removal
Introducing the secondary mixed gas at normal temperature into a methane absorption tank (3) by using a U-shaped pipe, wherein one end of the U-shaped pipe is inserted into the bottom of the methane absorption tank (3) to remove methane in the secondary mixed gas;
s4: carbon dioxide removal
Introducing the three-stage mixed gas into a carbon dioxide reaction kettle (4) by using a U-shaped pipe, wherein one end of the U-shaped pipe is inserted into the bottom of the carbon dioxide reaction kettle (4) to remove carbon dioxide in the three-stage mixed gas;
s5: two stage water vapor removal
And repeating S2, introducing the tertiary mixed gas into the quaternary mixed gas of the secondary cooler (5), cooling to 1-5 ℃, discharging high-purity hydrogen, and introducing into the gas collection tank (6).
2. A process for purifying hydrogen as claimed in claim 1, wherein: the chemical formula of the total reaction kettle (1) is CH4+ H2O = CO + H2, CO + H20= C02+3H2, the catalyst is nickel, the primary mixed gas is CH4, H2O, C02 and H2, and the concentration of hydrogen discharged from the device is 70-75%.
3. A process for purifying hydrogen as claimed in claim 1, wherein: the water vapor in the S1 is excessively filled and is 1.3-1.8 times of the natural gas amount, the reaction amount ratio of the initial natural gas to the water vapor is 1:1 for reaction, and the redundant natural gas is filled in by a subsequent filling mode.
4. A process for purifying hydrogen as claimed in claim 1, wherein: the first-stage mixed gas is CH4, H2, C02 and a large amount of water vapor, the second-stage mixed gas is CH4, C02 and H2 and a small amount of water vapor, the third-stage mixed gas is C02 and H2 and a small amount of water vapor, the fourth-stage mixed gas is H2 and a small amount of water vapor, and the concentration of H2 is 99.5-99.9%.
5. A process for purifying hydrogen as claimed in claim 1, wherein: the methane absorption tank is internally filled with (3) carbon tetrachloride solvent 2/3.
6. A process for purifying hydrogen as claimed in claim 1, wherein: the carbon dioxide reaction kettle (4) is filled with 2/3 limestone solution, and the reaction equation is CaCO3+ H2O + CO2= Ca (HCO3) 2.
7. A process for purifying hydrogen as claimed in claim 1, wherein: before each hydrogen purification, the vacuum-pumping treatment of the pipeline and the equipment is needed.
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| CN202010715872.1A CN111924803A (en) | 2020-07-23 | 2020-07-23 | Hydrogen purification process technology |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1170695A (en) * | 1996-06-24 | 1998-01-21 | 拜尔公司 | method for obtaining carbon monoxide and hydrogen |
| CN1360556A (en) * | 1999-07-09 | 2002-07-24 | 株式会社荏原制作所 | Process and apparatus for production of hydrogen by gasification of combustible material and method for electric generation using fuel cell and electric power generation system using fuel cell |
| CN1829656A (en) * | 2003-07-28 | 2006-09-06 | 犹德有限公司 | Method for extracting hydrogen from a gas containing methane, especially natural gas and system for carrying out said method |
| CN101190781A (en) * | 2006-11-23 | 2008-06-04 | 上海标氢气体技术有限公司 | Minitype light hydrocarbon steam reforming hydrogen manufacturing technique |
| US20100074839A1 (en) * | 2008-09-22 | 2010-03-25 | Raymond Francis Drnevich | Hydrogen production method |
-
2020
- 2020-07-23 CN CN202010715872.1A patent/CN111924803A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1170695A (en) * | 1996-06-24 | 1998-01-21 | 拜尔公司 | method for obtaining carbon monoxide and hydrogen |
| CN1360556A (en) * | 1999-07-09 | 2002-07-24 | 株式会社荏原制作所 | Process and apparatus for production of hydrogen by gasification of combustible material and method for electric generation using fuel cell and electric power generation system using fuel cell |
| CN1829656A (en) * | 2003-07-28 | 2006-09-06 | 犹德有限公司 | Method for extracting hydrogen from a gas containing methane, especially natural gas and system for carrying out said method |
| CN101190781A (en) * | 2006-11-23 | 2008-06-04 | 上海标氢气体技术有限公司 | Minitype light hydrocarbon steam reforming hydrogen manufacturing technique |
| US20100074839A1 (en) * | 2008-09-22 | 2010-03-25 | Raymond Francis Drnevich | Hydrogen production method |
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Application publication date: 20201113 |