CN101648698B - Preparation method of high purity hydrogen - Google Patents
Preparation method of high purity hydrogen Download PDFInfo
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- CN101648698B CN101648698B CN2009100182297A CN200910018229A CN101648698B CN 101648698 B CN101648698 B CN 101648698B CN 2009100182297 A CN2009100182297 A CN 2009100182297A CN 200910018229 A CN200910018229 A CN 200910018229A CN 101648698 B CN101648698 B CN 101648698B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a preparation method of hydrogen. The invention uses the hydrogen with the purity of 99.99% as raw material, adopts pressure and temperature pressure swing adsorption technology and utilizes the principle that the hydrogen separation coefficient of residual impurities in hydrogen such as N2, CH4 and the like is larger than that of the surface of adsorbents such as activated carbon, fine-pored silica gel and the like, to prepare hydrogen with the purity of more than 99.9999%. The process of the invention is characterized by energy-saving, environmental protection, safety, capability of large-scale production and convenient operation. The use of pressure and temperature pressure swing adsorption technology avoids the defect of the traditional technology that inert gas such as nitrogen and the like in hydrogen are hard to remove, no discharge of three wastes is appeared, the coexist of oxygen and hydrogen is precluded and the method is safer and more reliable.
Description
Technical field
The present invention relates to a kind of hydrogen (H
2) preparation technology, particularly a kind ofly utilize the methanol decomposition legal system to be equipped with high-purity hydrogen to be raw material, to carry out the secondarily purified method for preparing ultrapurity hydrogen.
Background technology
Raising day by day along with scientific and technological level, various technology, equipment, instrument are strengthened high-performance, highly sensitive electronic component dependency, and in the fabrication of electronic components process, during particularly semiconducter device is produced, material purity is its key, and material purity is constantly proposed higher requirement.Hydrogen is obligato reducing gas and shielding gas in the semi-conductor electricity sub-element is made, and therefore requires the hydrogen demand of purity constantly to increase to meeting electron production, and can not satisfy supply.The hydrogen (more than 99.9999%) of ultra-high purity must be provided, and the throughput of certain scale need be arranged.
The hydrogen of domestic production at present is mainly derived from water electrolysis hydrogen production gas, again and then purifying, owing to come from electrolytic process, inevitably consumes a large amount of electric energy and the oxygen association is arranged, and this exists simultaneously again and mixes the danger that generates explosion gases.The seventies, domestic absorption international advanced technology has been developed technology such as methanol decomposition reformation hydrogen production and preparing hydrogen by ammonia decomposition, and along with the maturation of methanol decomposition reforming hydrogen producing technology industrialized unit, to compare its superiority more and more obvious with traditional water electrolysis hydrogen production production.At first be with low cost, energy consumption reduces greatly, and compliance with environmental protection requirements avoids producing the oxygen of same quantity again, and its security is improved greatly.Along with improving constantly of reformation The Application of Technology and methyl alcohol pyrolysis catalytic agent performance, made conversion of methanol more than 98%.The hydrogen manufacturing cost is constantly reduced, in pure hydrogen preparation, adopted pressure swing adsorption, make hydrogen purity can reach 99.95-99.995%, created favourable basis, but its purity still can not satisfy the requirement in the manufacturing of semi-conductor electricity sub-element for hydrogen is further purified.N in the special hydrogen
2, CH
4To adopt other conventional methods be what be difficult for to remove Deng impurity, although the method for palladium diffusion is fully effectively, and the cost height, output is little, can not be used for high pressure and purify.Under the condition of routine, N
2, CH
4Almost all there are not adsorptivity or loading capacity very little to all sorbent materials.
Summary of the invention
In order to overcome the defective that above-mentioned production technology exists, the purpose of this invention is to provide a kind of method high-purity, ultra-pure hydrogen for preparing: is that raw material adopts transformation-alternating temperature adsorption technology with purity greater than 99.99% hydrogen, utilizes N residual in the pure hydrogen
2, CH
4Deng impurity under condition of ultralow temperature with adsorbent surfaces such as activated carbon, Kiselgel A with the bigger principle of hydrogen separation factor, the preparation 99.9999% above purity hydrogen.
Percentage ratio described in the present invention all is weight percentage except that specified otherwise is arranged.
Technical scheme of the present invention is: a kind of preparation method of high purity hydrogen may further comprise the steps:
(1) preparation of the pure hydrogen of unstripped gas
With methyl alcohol, pure water is raw material, is 240-275 ℃ in temperature, and pressure is under the 1.0Mpa, the Cu-series catalyst that adopts methanol steam reforming commonly used to use, and catalyse pyrolysis is mainly contained the reforming gas of hydrogen and carbonic acid gas; Hydrogen and carbonic acid gas reforming gas carry out the transformation fractionation by adsorption in adsorber, fill sorbent material in the adsorber to carbonic acid gas, methane, the selective absorption property of carbon monoxide, utilize transformation absorption (PSA) technology to extract pure hydrogen (purity＞99.99% from reforming gas,＜99.999%) foreign gas emptying after desorb.Described raw material CH
3OH and H
2The O mol ratio is 1: 1-1: 1.2, and the adsorption temp in the described pressure-swing adsorption process is a normal temperature, and adsorptive pressure is 1.0Mpa, and desorption pressures is 0.02Mpa.All identical except that specified otherwise is arranged among the preparation technology of the pure hydrogen of raw material with existing hydrogen production from methanol-steam reforming technology.
The production technology principle of described methanol steam catalyse pyrolysis hydrogen manufacturing is that methyl alcohol and steam mixture pressurized catalysis cracking in convertor were finished with one step of conversion, generates hydrogen and carbonic acid gas, and its reaction formula is as follows:
Main reaction: CH
3OH=CO+2H
2-90.7KJ/mol
CO+H
2O＝CO
2+H
2 +41.2KJ/mol
Total reaction: CH
3OH+H
2O=CO
2+ 3H
2-49.5KJ/mol
Side reaction: 2CH
3OH=CH
3OCH
3+ H
2O+24.90KJ/mol
CO+3H
2＝CH
4+H
2O
(2) transformation-alternating temperature adsorption cleaning
The pure hydrogen of raw material that obtains through step (1), earlier being compressed to pressure through membrane compressor is 13.0Mpa, successively purifying adsorber by de-oiling again is to remove micro oil under the sorbent material normal temperature with the activated carbon, sulphur compound, the deoxidizing purification reactor is that dehydrogenation catalyst is to remove the oxygen of trace under 20-400 ℃ through catalytic deoxidation in temperature with the palladium catalyst, through de-oiling, raw hydrogen behind sulphur compound and the oxygen is anhydrated for sorbent material normal temperature removes down with the molecular sieve through adsorption dehumifier after water cooler is chilled to normal temperature again, carbon monoxide and partial CO 2, tentatively lower the temperature through interchanger then, being sorbent material with activated carbon or Kiselgel A through the alternating temperature adsorber again removes nitrogen under temperature-185 ℃, the remaining carbonic acid gas of methane gas and part, obtain purity greater than 99.9999% ultra-pure hydrogen, foreign gas is emptying after desorb.Described transformation-alternating temperature adsorption cleaning equipment the desorb working pressure: 0.02MPa; The desorb service temperature is an activated carbon :-40 ℃, and molecular sieve: 200 ℃, palladium catalyst: 200-400 ℃.
Described ultra-pure hydrogen after purifying and the raw hydrogen heat exchange without denitrogenation gas and methane gas that is about to enter the alternating temperature adsorber have been played without the feed hydrogen cooling of denitrogenation gas and methane gas and the purpose that product hydrogen is heated up, described high product purity hydrogen will charge in the gas cylinder or be delivered to the scene of using, described liquid nitrogen is converted into after the gas phase recyclable or make high purity nitrogen after purifying, and it all be the adsorber of using always that the de-oiling in described transformation-alternating temperature adsorptive purifier purifies adsorber, deoxidizing purification reactor, adsorption dehumifier and alternating temperature adsorber.
The principle of work that de-oiling in the device is purified equipment such as adsorber, deoxidizing purification reactor, adsorption dehumifier, alternating temperature adsorber is summarized as follows:
1. de-oiling purifies adsorber
Raw material H
2Although carried out purifying, consider that beyond thought problem may take place in the upstream, for preventing the permanent poisoning (H of reductor
2Also may contain various sulfide), ad hoc have this adsorber, and its principle is to utilize activated carbon adsorbent that the physical adsorption of oil, sulphur compound is realized that de-oiling purifies.
2. deoxidizing purification reactor
H
2In O
2Must remove H
2Qi exhaustion oxygen is simple relatively, belongs to catalytic deoxidation, and its principle is to take place under the effect of catalyzer: 2H
2+ O
2=2H
2O.
3. adsorption dehumifier
Hydrogen through deoxidation contains certain water, carbon monoxide and carbonic acid gas, and these impurity are clean as if not handling, and can cause the downstream purification that ice takes place under liquid nitrogen temperature and block up, and makes regeneration temperature have to improve simultaneously.The sorbent material that adsorption dry is adopted is common molecular sieve.
4. alternating temperature adsorber
This device is that preparation is high-purity, the key equipment of ultra-pure hydrogen, is to utilize impurity N
2And CH
4, under liquid nitrogen temperature, with hydrogen the principle of separation factor is greatly arranged with activated carbon adsorbent or Kiselgel A adsorbent surface, remove above-mentioned residual impurity.
Technology of the present invention has the characteristics of energy-saving and environmental protection, safety, easy large-scale production and simple operation.The utilization of transformation-alternating temperature absorption has broken through the traditional technology that rare gas element such as nitrogen in the hydrogen is difficult to remove, and accomplishes three-waste free discharge, shut out anoxybioticly to exist simultaneously, and is safe more reliable.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
The raw hydrogen preparation: with methyl alcohol, pure water is raw material, is 268 ℃ in temperature, and pressure is under the 1.0Mpa, adopts the Cu-series catalyst catalyse pyrolysis mainly to be contained the reforming gas of hydrogen and carbonic acid gas; Hydrogen and carbonic acid gas reforming gas carry out the transformation fractionation by adsorption in adsorber, fill sorbent material in the adsorber to carbonic acid gas, methane, the selective absorption property of carbon monoxide, utilize transformation absorption (PSA) technology to extract pure hydrogen from reforming gas, described mol ratio is a methyl alcohol: water=1: 1.14, transformation adsorptive pressure 1MPa, desorption pressures is 0.02Mpa, adsorption temp: normal temperature, methyl alcohol unit consumption 0.61kg/Nm
3, the gained hydrogen purity:＞99.99%, the impurity and the content thereof of raw hydrogen are as shown in table 1.The production equipment of the pure hydrogen of described unstripped gas is to be made by Sichuan Yalian High-tech Co.,Ltd; The Cu-series catalyst that described methanol steam reforming uses is to be provided by Sichuan Yalian High-tech Co.,Ltd, and its model is AER601; The sorbent material to carbonic acid gas, methane, the selective absorption property of carbon monoxide of filling in the described adsorber is provided by Sichuan Yalian High-tech Co.,Ltd, and model is the II molecular sieve.
Foreign matter content (weight ratio) in the pure hydrogen unstripped gas of table 1
| Impurity component | Content (10 -6) |
| Nitrogen (N 2) | 40 |
| Oxygen (O 2) | 3.8 |
| Carbon monoxide (CO) | 4 |
| Carbonic acid gas (CO 2) | 4 |
| Methane (CH 4) | 5.2 |
| Water (H 2O) | 10 |
Hydrogen is secondarily purified: the raw hydrogen that obtains through step (1), earlier being compressed to pressure through membrane compressor is 13.0Mpa, successively purifying adsorber by de-oiling again is to remove micro oil under the sorbent material normal temperature with the activated carbon, sulphur compound, the deoxidizing purification reactor is that dehydrogenation catalyst is to remove the oxygen of trace under 82 ℃ through catalytic deoxidation in temperature with the palladium catalyst, through de-oiling, raw hydrogen behind sulphur compound and the oxygen is anhydrated for sorbent material normal temperature removes down with the molecular sieve through adsorption dehumifier after water cooler is chilled to normal temperature again, carbon monoxide and partial CO 2, tentatively lower the temperature through interchanger then, being sorbent material with the activated carbon through the alternating temperature adsorber again removes nitrogen under temperature-185 ℃, the remaining carbonic acid gas of methane gas and part, obtaining purity is greater than 99.9999% product hydrogen, feed hydrogen flow 12.8m
3/ h, impurity and content thereof in the product hydrogen are as shown in table 2.
Hydrogen impurity content (weight ratio) after table 2 is purified
| Impurity component | Content (10 -6) |
| Nitrogen (N 2) | 0.2 |
| Oxygen (O 2) | 0.1 |
| Carbon monoxide (CO) | 0.15 |
| Carbonic acid gas (CO 2) | 0.15 |
| Methane (CH 4) | 0.05 |
| Water (H 2O) | 2.0 |
Embodiment 2:
Raw hydrogen preparation: mol ratio: methyl alcohol: water=1: 1.15,271 ℃ of invert points, transfer pressure 1.0MPa, transformation adsorptive pressure 1.0MPa, desorption pressures are 0.02Mpa, adsorption temp is a normal temperature, methyl alcohol unit consumption 0.595kg/Nm
3, the gained hydrogen purity:＞99.99%, impurity and content thereof in the raw hydrogen are as shown in table 3, and all the other are with embodiment 1.
Foreign matter content (weight ratio) in the pure hydrogen unstripped gas of table 3
| Impurity component | Content (10 -6) |
| Nitrogen (N 2) | 52 |
| Oxygen (O 2) | 4 |
| Carbon monoxide (CO) | 3.6 |
| Carbonic acid gas (CO 2) | 2.8 |
| Methane (CH 4) | 3 |
| Water (H 2O) | 10 |
Hydrogen is secondarily purified: with the secondary-cleaned method of embodiment 1, obtain purity for greater than 99.9999% product hydrogen, feed hydrogen flow 12.8m
3/ h, impurity and content thereof in the product hydrogen are as shown in table 4.
Hydrogen impurity content (weight ratio) after table 4 is purified
| Impurity component | Content (10 -6) |
| Nitrogen (N 2) | 0.2 |
| Oxygen (O 2) | 0.05 |
| Carbon monoxide (CO) | 0.12 |
| Carbonic acid gas (CO 2) | 0.15 |
| Methane (CH 4) | 0.05 |
| Water (H 2O) | 1.5 |
Claims (1)
1. preparation method of high purity hydrogen may further comprise the steps:
(1) preparation of the pure hydrogen of unstripped gas: with methyl alcohol, pure water is raw material, is 240-275 ℃ in temperature, and pressure is under the 1.0MPa, and the Cu-series catalyst catalyse pyrolysis that adopts methanol steam reforming commonly used to use is mainly contained the reforming gas of hydrogen and carbonic acid gas; Hydrogen and carbonic acid gas reforming gas carry out the transformation fractionation by adsorption in adsorber, fill sorbent material in the adsorber to carbonic acid gas, methane, the selective absorption property of carbon monoxide, utilize pressure swing adsorption to extract and obtain purity greater than 99.99% from reforming gas, the pure hydrogen of raw material less than 99.999%, foreign gas is emptying after desorb, the mol ratio of described material benzenemethanol and pure water is 1: 1-1: 1.2, adsorption temp in the described pressure-swing adsorption process is a normal temperature, adsorptive pressure is 1.0MPa, and desorption pressures is 0.02MPa;
(2) transformation-alternating temperature adsorption cleaning: the pure hydrogen of raw material that obtains through step (1), earlier being compressed to pressure through membrane compressor is 13.0MPa, successively purifying adsorber by de-oiling again is to remove micro oil under the sorbent material normal temperature with the activated carbon, sulphur compound, the deoxidizing purification reactor is that dehydrogenation catalyst is to remove the oxygen of trace under 20-400 ℃ through catalytic deoxidation in temperature with the palladium catalyst, through de-oiling, raw hydrogen behind sulphur compound and the oxygen is anhydrated for sorbent material normal temperature removes down with the molecular sieve through adsorption dehumifier after water cooler is chilled to normal temperature again, carbon monoxide and partial CO 2, tentatively lower the temperature through interchanger then, being sorbent material with activated carbon or Kiselgel A through the alternating temperature adsorber again removes nitrogen under temperature-185 ℃, the remaining carbonic acid gas of methane gas and part, obtain purity greater than 99.9999% ultra-pure hydrogen, foreign gas is emptying after desorb, the desorb working pressure of described transformation-alternating temperature adsorption cleaning equipment: 0.02MPa, the desorb service temperature is: activated carbon :-40 ℃, molecular sieve: 200 ℃, palladium catalyst: 200-400 ℃.
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| CN102826509A (en) * | 2012-09-06 | 2012-12-19 | 浙江海天气体有限公司 | Equipment for purifying general hydrogen gas into high-purity hydrogen gas |
| CN102826509B (en) * | 2012-09-06 | 2015-02-18 | 浙江海天气体有限公司 | Equipment for purifying general hydrogen gas into high-purity hydrogen gas |
| CN108609583A (en) * | 2018-05-29 | 2018-10-02 | 四川天采科技有限责任公司 | A kind of LED-MOCVD processing procedures high concentration ammonia-containing exhaust warm journey pressure swing adsorption hydrogen production reuse method entirely |
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| CN101648698A (en) | 2010-02-17 |
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