CN101372314A - Method and apparatus for producing hydrogen from hydrogen-containing synthesis gas using palladium membrane - Google Patents
Method and apparatus for producing hydrogen from hydrogen-containing synthesis gas using palladium membrane Download PDFInfo
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- CN101372314A CN101372314A CNA2008100294635A CN200810029463A CN101372314A CN 101372314 A CN101372314 A CN 101372314A CN A2008100294635 A CNA2008100294635 A CN A2008100294635A CN 200810029463 A CN200810029463 A CN 200810029463A CN 101372314 A CN101372314 A CN 101372314A
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Abstract
The invention relates to a method which adopts a palladium membrane to produce high-purity hydrogen from hydrogen-containing synthetic gas and a device. In the method, synthetic gas which contains water vapor and hydrogen and is produced by an upstream hydrogen making reactor is firstly sent to a cooler, the cooled synthetic gas enters a gas-liquid separator, after dehydration, the synthetic gas enters a primary heater and is heated in the heater, the heated synthetic gas enters a secondary heater and heated to the temperature of 450-600 DEG C, the heated synthetic gas enters a palladium membrane separator, and most of hydrogen in the synthetic gas permeates the palladium membrane separator to become the high-purity finished hydrogen. A pipeline of the device which connects a heat exchanger and the palladium membrane separator is sequentially provided with the gas-liquid separator, the primary heater and the secondary heater, the palladium membrane separator is connected with a burner by the primary heater, and the burner is also connected with the secondary heater. The invention has simple design and high hydrogen separation efficiency of the palladium membrane and provides a new technical method for efficient production of high-purity hydrogen.
Description
Technical field:
The present invention relates to a kind of technology of from hydrogen containing synthesis gas, producing high-purity hydrogen, specially refer to the method and apparatus that utilizes the palladium membrane sepn to prepare high-purity hydrogen.
Background technology
Present 90% hydrogen in the world comes from the reformation of hydrocarbon polymer (Sweet natural gas, coal, biomass etc.), obtains through purifying after the chemical processes such as gasification or cracking, and the purification of synthetic gas is one of them crucial technological process.The available purification techniques has: transformation absorption, polymeric membrane separates, palladium membrane sepn, low ternperature separation process etc.Compare with other isolation technique, the palladium membrane sepn can be produced the high-purity hydrogen that only contains ppb rank impurity, especially adapts to the requirement of fuel cell; The occupation of land of palladium membrane separation unit is little in addition, and is also easy than other several separation methods aspect miniaturization.
So-called " dissolving-diffusion " (Solution-diffusion) mechanism is obeyed in the transmission of hydrogen in the palladium film, and it comprises following process: hydrogen is diffused into palladium film surface from the frictional belt; Hydrogen resolves into hydrogen atom on the film surface; Hydrogen atom is dissolved by the palladium film; Hydrogen atom is diffused into low-tension side from the high-tension side in the palladium film; Hydrogen atom stresses newly to synthesize hydrogen molecule at the palladium film at low pressure; The film surface is left in the hydrogen diffusion.According to above-mentioned theory, the penetration coefficient of hydrogen in the palladium film and the temperature of film, thickness, alloying constituent, and hydrogen is relevant in the dividing potential drop of film both sides, and available Sievert ' s Law expresses:
In the formula:
R: gas law constant; T: temperature; A: membrane area; L: film thickness; E: activation energy; P
h: hydrogen high-tension side dividing potential drop; P
l: hydrogen low-tension side dividing potential drop; N: pressure index; K: coefficient before the exponential function; M: transmitance.
The method that the using palladium membrane sepn is produced hydrogen mainly contains two kinds: A) membrane module and hydrogen-manufacturing reactor being coupled as one becomes membrane reactor, utilizes this reactor single stage method to obtain highly purified hydrogen through reacting with separating from unstripped gas.The coupling of membrane sepn and reaction process can be broken the thermodynamic(al)equilibrium of reaction, makes that reaction helps carrying out to the direction of producing hydrogen.But owing to increased membrane separation assemblies in the reactor, and the structure of reactor complexity, the palladium film directly contacts with reaction medium and catalyzer, and operational conditions is more abominable, and the palladium membrane lifetime is shorter.B) the palladium membrane sepn separates with hydrogen-manufacturing reactor, hydrogen-manufacturing reactor production hydrogen containing synthesis gas, and its downstream adopts the palladium membrane sepn to obtain high-purity hydrogen, and this method technology is simple, and operating maintenance is all more convenient.Produce in the technology of synthetic gas at the hydrocarbon polymer steam reformation of industrial widespread use, in order to prevent the transformation efficiency of catalyst carbon deposition and raising hydrocarbon polymer, water vapor often is excessive greatly, causes the water vapor that contains in the synthetic gas more than 30%.By Sievert ' the s Law of palladium membrane sepn as can be known, the power of palladium membrane sepn mainly comes to have by oneself the difference of the inside and outside hydrogen partial pressure of film, and under the situation that the synthetic gas total pressure remains unchanged, the existence of a large amount of water vapors in the synthetic gas, greatly reduce the dividing potential drop of hydrogen in the synthetic gas, thereby reduced the efficient that membrane sepn is produced hydrogen.As shown in Figure 2, the synthetic gas that traditional direct membrane separation process, upstream hydrogen-manufacturing reactor generate directly by the road P21 be introduced into interchanger 1 heat exchange to membrane separation apparatus working temperature (450-600 ℃); Come out by the road from interchanger 1 that P22 enters membrane separation apparatus 5, product hydrogen is transported to the downstream by pipeline P23, and tail gas is transported to burner 6 burnings by pipeline P24, and the flue gas that is produced 26 is transported to the upstream and produces water vapor by the road.There is the problem of two aspects in this technology, and the one, water vapour content height in the mixed gas reduces palladium membrane sepn efficient.The 2nd, heat energy can not effectively utilize, the energy consumption height.
Summary of the invention
The shortcoming that the objective of the invention is to the customer service prior art provides a kind of Hydrogen Separation efficient height, the energy-conservation palladium film that utilizes to produce the method for high-purity hydrogen from hydrogen containing synthesis gas.
Another object of the present invention is to provide realization the above-mentioned device that utilizes the palladium film from hydrogen containing synthesis gas, to produce the high-purity hydrogen gas method.
Purpose of the present invention is achieved through the following technical solutions:
A kind of method of utilizing the palladium film to produce high-purity hydrogen from hydrogen containing synthesis gas comprises the steps:
(1) synthetic gas that contains water vapor and hydrogen from upstream hydrogen-manufacturing reactor production at first enters water cooler, is reduced to 75～85 ℃, and the synthetic gas after the cooling enters gas-liquid separator, realizes separating with synthetic gas behind the water vapor condensation;
(2) synthetic gas after dewatering enters primary heater, and synthetic gas is heated to 250～350 ℃ in well heater, and the heating medium of well heater is for going out the high-temperature tail gas behind the hydrogen through the palladium membrane sepn; Be heated the back synthetic gas and enter secondary heater, synthetic gas is heated to 450～600 ℃, and heating medium is the formed flue gas of exhaust combustion through primary heater;
(3) heated synthetic gas enters the palladium membrane separation apparatus, and the most of hydrogen in the synthetic gas sees through the palladium membrane separation apparatus becomes high purity product hydrogen; High-temperature tail gas enters the synthetic gas after the primary heater heating dewaters.
The medium of described step (1) heat exchange is a cold water, and cold water becomes water vapor after heat exchange, as the process water steam of upstream carbon hydrogen compound reformation usefulness.
Utilize the palladium film from hydrogen containing synthesis gas, to produce the device of high-purity hydrogen, comprise interchanger, palladium membrane separation apparatus, burner, described interchanger is connected with the palladium membrane separation apparatus, the palladium membrane separation apparatus is connected with burner, it is characterized in that: be provided with gas-liquid separator, primary heater and secondary heater successively on the pipeline of described connection interchanger and palladium membrane separation apparatus, described palladium membrane separation apparatus is connected with burner by primary heater, and described burner also is connected with secondary heater.
The present invention is directed to independent employing palladium membrane separation apparatus when from hydrogen containing synthesis gas, producing high-purity hydrogen, a large amount of water vapors in the synthetic gas reduce the situation of palladium membrane sepn efficient, adopt interchanger to reduce the temperature of synthetic gas, thereby the vapour content in the reduction synthetic gas reheats the synthetic gas after dewatering and enters the palladium membrane separation apparatus and produce high-purity hydrogen.Simplicity of design of the present invention, palladium membrane sepn hydrogen efficient height is for the High-efficient Production high-purity hydrogen provides a kind of new processing method.
The technology that existing membrane sepn is produced hydrogen is compared, and the present invention has following advantage:
(1) hydrogen containing synthesis gas was removed a large amount of water vapors that contain in the synthetic gas before entering membrane separation apparatus, had improved the efficient of membrane sepn.Compare with traditional technology, under same hydrogen yield, can reduce and separate required membrane area, save cost.
(2) the present invention adopts the integrated mode of energy in the water vapor in removing synthetic gas, utilize the required water vapor of high-temperature synthesis gas production upstream hydrogen production process, and utilize the sensible heat of tail gas of palladium membrane separation apparatus and the combustion heat to heat synthetic gas after dewatering, improved energy utilization efficiency.
Description of drawings
Fig. 1 utilizes the palladium film to produce the device synoptic diagram of high-purity hydrogen from hydrogen containing synthesis gas.
Fig. 2 is tradition is directly produced high-purity hydrogen with the palladium membrane sepn a device synoptic diagram.
Embodiment
In order to understand technical scheme of the present invention better, further specify the present invention below in conjunction with embodiment and accompanying drawing, need to prove that embodiment does not constitute the qualification to protection domain of the present invention.
As shown in Figure 1, utilize the palladium film from hydrogen containing synthesis gas, to produce the device of high-purity hydrogen, comprise water cooler 1, gas-liquid separator 2, primary heater 3, secondary heater 4, palladium membrane separation apparatus 5 and burner 6.Pipeline P01, P02, P04, the P06 of circulation hydrogen containing synthesis gas connect water cooler 1, gas-liquid separator 2, primary heater 3, secondary heater 4 and palladium membrane separation apparatus 5 successively; The water coolant of water cooler 1 is entered by pipeline P13, is flowed out by pipeline P14.Isolated water of condensation is discharged by pipeline P03 in the gas-liquid separator 2.High-purity 1 hydrogen that palladium membrane separation apparatus 5 is produced is drawn by pipeline P07, and tail gas is connected to primary heater 3 and burner 6 successively by pipeline P08, P09.The pipeline P10 air that burner 6 burning is required is introduced, and the high-temperature flue gas that burner 6 burnings are produced is introduced secondary heater 4 by pipeline P11, and is connected to the downstream by pipeline P12 and utilizes once more.
Embodiment: the separation of hydrogen is purified in the multikilowatt fuel cell hydrogen-feeding system
The hydrogen source of Proton Exchange Membrane Fuel Cells needs the very high hydrogen of purity, content to CO has very high requirement especially, utilize the palladium membrane sepn can obtain the pure hydrogen of impurity, and palladium membrane sepn volume is little, is fit to be applied to the small home fuel cell plant for the ppb level.
Synthetic gas is produced by the gas water steam reforming reaction, and reactor can be conventional fixed-bed reactor, or novel fluidized bed reactor, micro passage reaction etc.Synthetic gas consists of the gas composition of reacting when reaching balance.The reaction raw materials airshed is as follows: Sweet natural gas (pressing methanometer): 0.280kg/h, water vapor: 0.944kg/h, temperature of reaction: 700 ℃; Reaction pressure: 1.1MPa; Then its outlet (P01) synthetic gas molar constituent is as follows: CH4:7.9%; H
2O:39.5%; H
2: 41.2%; CO:4.5%; CO
2: 69%; As seen the water vapor that contains nearly 40% volume of having an appointment in the synthetic gas, hydrogen partial pressure are 0.453MPa.
Adopt Hydrogen Separation flow process shown in Figure 1.Process datas such as the temperature of employing ASPEN Plus software simulation scaling system 1 each pipeline section medium, pressure, as shown in table 1.
In this example,, increase hydrogen partial pressure, at first the synthetic gas among the pipeline P01 is fed water cooler 1 for reducing vapour content.Under this water cooler device 1 effect, the synthetic gas temperature is reduced to 83 ℃.The medium of heat exchange is a cold water, and this cold water becomes water vapor after heating, the process water steam of using as the natural gas upstream steam reforming reaction.Water cooler is selected shell and tube heat exchanger for use, and synthetic gas enters shell side, and water coolant is walked tube side, heat interchanging area: 0.0027m
2, heat is 0.62kw.
Synthetic gas after the cooling enters gas-liquid separator 2 by pipeline P02, and 90% water separates from gas-liquid separator in the synthetic gas, and water of condensation is discharged by pipeline P03.Gas-liquid separator is a pressurized vessel, and material is selected the stainless steel into 316L for use, design pressure 1.2MPa: 100 ℃ of design temperatures are equipped with automatic pumping equipment.
Hydrogen volume content in the synthetic gas after dewatering increases to 65.0% by 41.2%, and it is 0.715MPa that dividing potential drop is raise by 0.453MPa, enters primary heater 3 by pipeline P04, and synthetic gas is heated to 324 ℃.The heating medium of well heater is the high-temperature tail gas after process palladium membrane sepn goes out hydrogen, and exhaust temperature is reduced to 180 ℃ by 600 ℃.Primary heater 3 is selected double-pipe exchanger for use, and synthetic gas enters shell side, and high-temperature tail gas is walked tube side, heat interchanging area 0.009m
2, heat 0.128kw.
The synthetic gas that leaves primary heater 3 enters secondary heater 4 by pipeline P05, and synthetic gas is heated to 600 ℃ in this well heater.The heating medium of well heater is the formed flue gas of exhaust combustion through primary heater 3, and flue-gas temperature is reduced to 765 ℃ by 1000 ℃.Well heater 4 adopts double-pipe exchanger, and synthetic gas enters shell side, and high-temperature flue gas is walked tube side, heat interchanging area 0.00043m
2
The hydrogen containing synthesis gas that is heated to 600 ℃ enters palladium membrane separation apparatus 5 by pipeline P06.At this, the most of hydrogen in the synthetic gas sees through the palladium membrane separation apparatus becomes high purity product hydrogen.Palladium membrane separation apparatus 5 is a pressurized vessel that includes palladium membrane component (introducing as Chinese invention patent application 200710031743.5), Vessel Design pressure 1.2MPa: 650 ℃ of design temperatures.Palladium film in the palladium membrane component adopts palladium (75%) silver (25%) alloy film, film thickness 25 μ m, membrane area 0.018m
2, hydrogen output 0.06kg/h, hydrogen recovery rate 80%.
The tail gas of removing most of hydrogen in the palladium membrane separation apparatus 5 enters primary heater 3 by pipeline P08, and temperature is reduced to 180 ℃, enters burner 6 burnings by pipeline P09.High-temperature flue gas after the burning enters secondary heater 4 heating hydrogen containing synthesis gas by pipeline P11, and temperature is reduced to 765 ℃ by 1000 ℃, and low-temperature flue gas is sent into the upstream hydrogen generating system by pipeline P12, can be hydrogen-manufacturing reactor heat is provided.
If adopt traditional as shown in Figure 2 direct membrane separation process, the synthetic gas that the upstream hydrogen-manufacturing reactor generates directly by the road P21 be introduced into water cooler 1 and be cooled to optimal working temp 450-600 ℃ of membrane separation apparatus; Come out by the road from water cooler 1 that P22 enters membrane separation apparatus 5, hydrogen is transported to the downstream by pipeline P23, and tail gas is transported to burner 6 burnings by pipeline P24, and the flue gas that is produced 26 is transported to the upstream and produces water vapor by the road.Pipeline P25 introduces the required air of burner 6 burnings.If identical among the composition of the synthetic gas among the pipeline P21 and Fig. 1 among the P01 then will reach hydrogen output 0.06kg/h same with the above-mentioned embodiment, needed total membrane area is 0.046m
2, comparing with traditional membrane separation process, the present invention can be reduced to the palladium membrane area original 39%.
By above-mentioned contrast as can be seen,, can effectively remove the water component in the synthetic gas, improve the dividing potential drop of hydrogen in the synthetic gas, thereby improve the efficient of membrane sepn by entering the synthetic gas refrigerative method of membrane separation apparatus.
Claims (7)
1. a method of utilizing the palladium film to produce high-purity hydrogen from hydrogen containing synthesis gas is characterized in that comprising the steps:
(1) synthetic gas that contains water vapor and hydrogen from upstream hydrogen-manufacturing reactor production at first enters water cooler, is reduced to 75～85 ℃, and the synthetic gas after the cooling enters gas-liquid separator, separates with synthetic gas behind the water vapor condensation;
(2) synthetic gas after dewatering enters primary heater, and synthetic gas is heated to 250～350 ℃ in well heater, and the heating medium of well heater is for going out the high-temperature tail gas behind the hydrogen through the palladium membrane sepn; Be heated the back synthetic gas and enter secondary heater, synthetic gas is heated to 450～600 ℃, and heating medium is the formed flue gas of exhaust combustion through primary heater;
(3) heated synthetic gas enters the palladium membrane separation apparatus, and the most of hydrogen in the synthetic gas sees through the palladium membrane separation apparatus becomes high purity product hydrogen; High-temperature tail gas enters the synthetic gas after the primary heater heating dewaters.
2. the method for utilizing the palladium film from hydrogen containing synthesis gas, to produce high-purity hydrogen according to claim 1, it is characterized in that: the medium of described step (1) heat exchange is a cold water, cold water becomes water vapor after heat exchange, as the process water steam of upstream carbon hydrogen compound reformation usefulness.
3. the palladium film that utilizes of realizing the described method of claim 1 is produced the device of high-purity hydrogen from hydrogen containing synthesis gas, comprise interchanger, palladium membrane separation apparatus, burner, described interchanger is connected with the palladium membrane separation apparatus, the palladium membrane separation apparatus is connected with burner, it is characterized in that: be provided with gas-liquid separator, primary heater and secondary heater successively on the pipeline of described connection interchanger and palladium membrane separation apparatus, described palladium membrane separation apparatus is connected with burner by primary heater, and described burner also is connected with secondary heater.
4. the device that utilizes the palladium film to produce high-purity hydrogen from hydrogen containing synthesis gas according to claim 3 is characterized in that: described water cooler is telescoping, board-like, shell and tube or tube and shell heat exchanger.
5. the device that utilizes the palladium film to produce high-purity hydrogen from hydrogen containing synthesis gas according to claim 3 is characterized in that: described primary heater is telescoping, board-like, shell and tube or tube and shell heat exchanger.
6. the device that utilizes the palladium film to produce high-purity hydrogen from hydrogen containing synthesis gas according to claim 3 is characterized in that: described secondary heater is telescoping, board-like, shell and tube or tube and shell heat exchanger.
7. the device that utilizes the palladium film to produce high-purity hydrogen from hydrogen containing synthesis gas according to claim 3 is characterized in that: described burner is atmospheric burner or Flameless burner.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102328906A (en) * | 2011-07-18 | 2012-01-25 | 中国科学院大连化学物理研究所 | Recycling hydrogen purification processing method for producing polysilicon by reducing trichlorosilane |
| CN104129758A (en) * | 2014-08-19 | 2014-11-05 | 中国工程物理研究院核物理与化学研究所 | Hydrogen isotope exchange membrane reaction assembly |
| CN110526211A (en) * | 2019-09-25 | 2019-12-03 | 浙江高成绿能科技有限公司 | A kind of portable chemical hydrogen generating system |
| CN112062088A (en) * | 2019-06-11 | 2020-12-11 | 义乌市锐胜新材料科技有限公司 | Hydrogen separation system for alcohol reforming hydrogen production |
| CN113252591A (en) * | 2021-06-15 | 2021-08-13 | 佛山绿色发展创新研究院 | Detection system and detection method applied to hydrogen distribution station |
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| CN2266586Y (en) * | 1996-10-26 | 1997-11-05 | 中国科学院山西煤炭化学研究所 | Self-supplying heat palladium film separation high purity hydrogen generator |
| CN100469417C (en) * | 2005-03-15 | 2009-03-18 | 大连欧科膜技术工程有限公司 | System for recovering hydrogen from air of methanol synthesis processing by membrane method |
| CN201301223Y (en) * | 2008-07-15 | 2009-09-02 | 华南理工大学 | Palladium membrane module device for producing high-purity hydrogen from hydrogen-contained synthesis gas |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102328906A (en) * | 2011-07-18 | 2012-01-25 | 中国科学院大连化学物理研究所 | Recycling hydrogen purification processing method for producing polysilicon by reducing trichlorosilane |
| CN102328906B (en) * | 2011-07-18 | 2014-02-12 | 中国科学院大连化学物理研究所 | Recycling hydrogen purification processing method for producing polysilicon by reducing trichlorosilane |
| CN104129758A (en) * | 2014-08-19 | 2014-11-05 | 中国工程物理研究院核物理与化学研究所 | Hydrogen isotope exchange membrane reaction assembly |
| CN104129758B (en) * | 2014-08-19 | 2015-10-21 | 中国工程物理研究院核物理与化学研究所 | A kind of hydrogen isotopic exchange film reaction assembly |
| CN112062088A (en) * | 2019-06-11 | 2020-12-11 | 义乌市锐胜新材料科技有限公司 | Hydrogen separation system for alcohol reforming hydrogen production |
| CN110526211A (en) * | 2019-09-25 | 2019-12-03 | 浙江高成绿能科技有限公司 | A kind of portable chemical hydrogen generating system |
| CN110526211B (en) * | 2019-09-25 | 2024-03-29 | 浙江高成绿能科技有限公司 | Portable chemical hydrogen production system |
| CN113252591A (en) * | 2021-06-15 | 2021-08-13 | 佛山绿色发展创新研究院 | Detection system and detection method applied to hydrogen distribution station |
| CN113252591B (en) * | 2021-06-15 | 2021-10-15 | 佛山绿色发展创新研究院 | Detection system and detection method applied to hydrogen distribution station |
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| CN101372314B (en) | 2011-04-27 |
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