CN102806001B - Method and device for selectively removing hydrogen sulfide by use of ultrasonically atomized liquid droplets - Google Patents

Method and device for selectively removing hydrogen sulfide by use of ultrasonically atomized liquid droplets Download PDF

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CN102806001B
CN102806001B CN201210339435.XA CN201210339435A CN102806001B CN 102806001 B CN102806001 B CN 102806001B CN 201210339435 A CN201210339435 A CN 201210339435A CN 102806001 B CN102806001 B CN 102806001B
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drop
hydrogen sulfide
gas
cyclone
methyl diethanolamine
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CN102806001A (en
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钱鹏
汪华林
许德建
吴精平
邱阳
吴文峰
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Shanghai Huachang Environmental Protection Co Ltd
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Abstract

The invention relates to a method and device for selectively removing hydrogen sulfide by use of ultrasonically atomized liquid droplets, and provides a method for selectively removing hydrogen sulfide by use of ultrasonically atomized liquid droplets. The method comprises (i) atomizing a methyldiethanolamine solution by ultrasonic atomization to give liquid droplets with a size of 10-15mum; (ii) uniformly mixing the obtained methyldiethanolamine liquid droplets with a gas containing hydrogen sulfide and spraying the mixture into a cyclone within time shorten than one second; (iii) in the cyclone, allowing the methyldiethanolamine liquid droplets to absorb the hydrogen sulfide in the gas while separating the methyldiethanolamine liquid droplets in the cyclone field of the cyclone, and aggregating to form a hydrogen sulfide-rich methyldiethanolamine solution; and (iv) recycling the hydrogen sulfide-rich methyldiethanolamine solution, atomizing by ultrasonic atomization to give liquid droplets, and cyclically using the liquid droplets in the step (ii). Also provided is a device for selectively removing hydrogen sulfide by use of ultrasonically atomized liquid droplets.

Description

The method and apparatus of ultrasonic atomizatio drop selective desulfurization hydrogen
Technical field
The invention belongs to chemical industry environmental protection field, relating to a kind of ultrasonic ultrasonic delay line memory that adopts is drop by methyl diethanolamine atomization, selectively removing hydrogen sulfide in cyclone, and drop is isolated in eddy flow field, be purified the method for gas, be suitable for processing the selective desulfurization and solution-air heterogeneous separation process that comprise the sour gas such as sulfide hydrogen, carbon dioxide.Specifically, the invention provides selective desulfurization in H 2 S-containing gas sulfur removal technology, absorb the cyclonic separation method and apparatus of drop.
Background technology
Along with the development of economic society, the air pollution that combustion of fossil fuel causes and greenhouse effects seriously threaten the earth environment that the mankind depend on for existence, in the process utilizing fossil feedstock, and inorganic sulfur (hydrogen sulfide, SO 2deng) and the factor arranged into have the greatest impact to earth environment of carbon dioxide.
According to absorbing and removing Principle of Process, current desulfurization and decarburization separation method mainly contains: absorption process, absorption method, membrane separation process etc.Wherein in chemical absorption method, hydramine method and hot potash method become the dominant absorption method that a large amount of sulfur-bearing carbon containing gaseous mixture discharges in the main energy sources class manufacturers such as petrochemical industry, Coal Chemical Industry, power plant.The equipment of usual employing is the equipment such as packed tower, spray column or plate column, and desulfurization and decarburization agent, mainly with relatively large solution state and gas haptoreaction, causes contact area few, and solvent use amount is large, the shortcomings such as efficiency is not high.And owing to absorbing sour gas by tower, there is mass transfer effect difference, energy consumption is large, equipment volume is huge, one-time investment cost is high, the problems such as fluctuation of service.
Therefore, current sulfurous gas purification techniques means are unsatisfactory for the selective desulfurization effect of the sour gas such as sulfide hydrogen and carbon dioxide, in multiple sour gas, effectively, optionally can not remove hydrogen sulfide gas, this is also problem in urgent need to solve in the field gas purifications such as current natural gas production.
Chinese patent application CN 200710020017.3 discloses a kind of gas absorption purifier, and equipment is a vertical cylinder, and after entering tower by allowing pending gas, one side rotates one side along flight and rises, and contacts with absorbing liquid is reverse; Absorbing liquid forms liquid film, brin and drop under the turbulent shear effect of eddy flow field, makes gas-liquid fully contact absorption.But only rely on gas-liquid collision fragmentation that absorbing liquid cannot be made completely fully broken, and size droplet diameter is very large, haptoreaction limited area, cannot reach good assimilation effect.
Chinese patent application CN 01242489.7 discloses a kind of toxic and harmful absorbing and purifying device, arranges bilevel absorbing liquid shower nozzle in absorption tower, is sprayed into the toxic gas of drop absorption.But this device does not still break away from tower, the large investment of volume is large, and the drop of shower nozzle ejection still exists the excessive factor of size droplet diameter, causes absorbing liquid to waste.
Chinese patent application 200910051410.8 discloses a kind of eddy flow intensifying method and device of gas sweetening hydrogen, the method first carries out cyclonic separation to fuel gas gaseous mixture, to remove the heavy hydrocarbon component wherein carried secretly, again desulfurization is carried out to the gaseous mixture being stripped of heavy hydrocarbon component, to remove the 2 S component wherein carried secretly, be purified gas.But absorb in the method for this depriving hydrogen sulphide or traditional desulfurizing tower, absorbing liquid use amount is large, and absorbs non-selectivity to sour gas.
Therefore, for meeting environmental requirement, reduce solvent use amount and improve absorption efficiency, being necessary the feature can carrying out selective absorbing for the sulfide hydrogen such as natural gas, refinery gas sour gas, develop a kind of novelty, effectively, the selective desulfurization method of good economy performance.
Summary of the invention
The invention provides a kind of method and apparatus of ultrasonic atomizatio drop selective desulfurization hydrogen of novelty, thus solve problems of the prior art.
The object of the invention is to, propose one and utilize the method such as ultrasonic atomization or spraying, produce methyl diethanolamine drop, strengthening gas-selectively hydrogen sulfide removal process, improves separative efficiency, reduces equipment volume, save methyl diethanolamine use amount, thus solve problems of the prior art.
Primary technical problem to be solved by this invention is, solve desulfuration selectivity in existing H 2 S-containing gas removing process not strong, absorption efficiency is low, causes the problem that methyl diethanolamine is wasted, and improves absorption efficiency and absorbs precision.
Another technical problem that the present invention also solves simultaneously is, provide a kind of desulfurizer with above-mentioned efficient selective sulfur method, this apparatus structure is simple, easy enforcement, meet desulphurization plant design specification, can operate by stability and high efficiency, be especially applicable to H 2 S-containing gas and depart from the feature that in technique, treating capacity is large, gas componant is complicated.
On the one hand, the invention provides a kind of method of ultrasonic atomizatio drop selective desulfurization hydrogen, the method comprises the following steps:
(i) utilize ultrasonic atomization by methyldiethanolamine solution atomization for particle diameter is the drop of 10-50 μm;
(ii) the methyl diethanolamine drop of gained is mixed with hydrogen sulfide containing gas uniform, and within the time being no more than 1 second, mixture is sprayed in cyclone;
(iii) in cyclone, the hydrogen sulfide in methyl diethanolamine drop absorption gas, methyl diethanolamine drop is separated in the eddy flow field of cyclone simultaneously, and assembles the rich hydrogen sulfide containing methyl diethanolamine liquid of formation; And
(iv) after rich hydrogen sulfide containing methyl diethanolamine liquid regeneration, then be drop by it by ultrasonic atomization atomization, and the drop of gained is cycled to used in above-mentioned steps (ii) in.
In one preferred embodiment, described hydrogen sulfide containing gas contains hydrogen sulfide and carbon dioxide, and wherein the concentration of hydrogen sulfide is between 100-10000ppm.
Another preferred embodiment in, in cyclone, hydrogen sulfide containing gas and the abundant haptoreaction of methyl diethanolamine drop, hydrogen sulfide is fully absorbed by methyl diethanolamine drop, and absorptivity is higher than 99.5%.
Another preferred embodiment in, in cyclone, methyl diethanolamine drop and hydrogen sulfide containing gas carry out cyclonic separation simultaneously, and methyl diethanolamine drop is separated in the eddy flow field of cyclone, separative efficiency is higher than 90%, and maximum pressure falls and is not more than 30mmH 2o.
On the other hand, the invention provides a kind of device of ultrasonic atomizatio drop selective desulfurization hydrogen, this device comprises:
Ultrasonic ultrasonic delay line memory, for by methyldiethanolamine solution atomization for particle diameter is the drop of 10-50 μm;
In pipe, bottom arranges the droplet distribution pipe of ultrasonic ultrasonic delay line memory, for being mixed with hydrogen sulfide containing gas uniform by the methyl diethanolamine drop of gained;
The cyclone be connected with droplet distribution pipe, is provided for the hydrogen sulfide in methyl diethanolamine drop absorption gas, and methyl diethanolamine drop is separated in the eddy flow field of cyclone simultaneously, and assembles the rich hydrogen sulfide containing methyl diethanolamine liquid of formation.
In one preferred embodiment, described droplet distribution pipe is connected to gas feed, gas is entrained with methyl diethanolamine drop and enters in cyclone in pipe, and methyl diethanolamine drop fully contacts absorption with the hydrogen sulfide in gas, and in the gas after desulfurization, the concentration of hydrogen sulfide is less than 20ppm.
Another preferred embodiment in, the reaction of methyl diethanolamine drop absorption hydrogen sulfide is carried out under Elevated Gravity, and the haptoreaction time is less than 0.1 second.
Another preferred embodiment in, described cyclone also carries out the gas-liquid separation of methyl diethanolamine drop and hydrogen sulfide gas simultaneously, and purified gas is discharged from the overfall of cyclone, drop enrichment enter amine liquid regenerating unit regeneration Posterior circle utilize.
Another preferred embodiment in, the quantity of described ultrasonic ultrasonic delay line memory is one or more.
Another preferred embodiment in, the quantity of described cyclone is one or more.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the ultrasonic atomization drop selective desulfurization hydrogen technique of an embodiment according to the application.
Fig. 2 is the schematic diagram carrying out contact mass transfer reaction according to gas of the present invention and drop.
Detailed description of the invention
The present inventor finds after have passed through extensive and deep research: in current process equipment, carry out because solution-air two-phase haptoreaction is also in a very large yardstick, absorption efficiency is low, methyl diethanolamine utilization rate is low, the large investment of equipment volume is large, and how fluctuation of service, therefore, carry out reinforcing desulfuration process just more and more concerned in industrial research in the following yardstick of small scale, even micron order; Adopt at present both at home and abroad extensively hydramine method etc. as sulfur method, how the absorption reaction of hydramine to be become micron level, thus improve absorption efficiency, reach the fast selective desulfurization object economized; From this angle, the present inventor proposes and adopts droplet method to strengthen selective desulfurization process;
As shown in Figure 2, gas-liquid mass transferring reaction mainly overcomes resistance between gas liquid film, in the present invention, methyl diethanolamine contacts with sulfur-bearing carbon containing gaseous mixture with microlayer model form, substantially increase contact surface area, gaseous mixture fully can contact microlayer model at a terrific speed, carries out reactive absorption; And reaction speed and absorption efficiency, with its microlayer model composition, gas componant, relevant containing sulphur concentration, reaction temperature pressure etc.;
By ultrasonic ultrasonic delay line memory, methyl diethanolamine is atomized as drop, considerably increases gas liquid interfacial area and hydrogen sulfide absorption efficiency; The gas of entrained drip carries out the solution-air cyclonic separation of low pressure drop simultaneously, and separative efficiency can reach more than 90%; So both complete the coupling that desulphurization reaction and eddy flow take off liquid, improve the utilization ratio of methyl diethanolamine, saved cost and subsequent regeneration energy consumption, make again the volume of industrial equipment reduce, reduce manufacturing cost.Based on above-mentioned discovery, the present invention is accomplished.
In a first aspect of the present invention, provide a kind of method of ultrasonic atomizatio drop selective desulfurization hydrogen, the method comprises:
Utilize ultrasonic ultrasonic delay line memory by methyldiethanolamine solution atomization for particle diameter is the drop of 10-50 μm;
Methyl diethanolamine drop is mixed with hydrogen sulfide containing gas uniform, within the time being no more than 1 second, sprays in cyclone;
In cyclone, the hydrogen sulfide in methyl diethanolamine drop absorption gas, methyl diethanolamine drop is separated in the eddy flow field of cyclone simultaneously, and assembles the rich hydrogen sulfide containing methyl diethanolamine liquid of formation;
After rich amine solution regeneration, then be drop by the atomization of mixture ultrasonic ultrasonic delay line memory, and recycle.
In the present invention, be provided with methyl diethanolamine drop generation systems and cyclone, be optionally stripped of the hydrogen sulfide in gaseous mixture, isolate the drop after absorbing simultaneously, thus the technological process completing absorption efficiently, once, be separated.
In the present invention, the concentration of described methyldiethanolamine solution is 20-80%, and operating temperature is 20-120 DEG C.
In the present invention, in described gaseous mixture, the concentration of hydrogen sulfide is between 100-10000ppm, SO 2content is not more than 5%, and carbon dioxide content is not more than 30%.
In the present invention, the sour gas composition in gaseous mixture is carbon dioxide, CO, SO 2, NO x, and the mixture of one or more gases above-mentioned.
In the present invention, the quantity of methyl diethanolamine drop generation systems and cyclone and arrangement, can according to condition appropriate design such as the tolerance of gaseous mixture air inlet, pressure, compositions.
In the present invention, the treating capacity of described ultrasonic ultrasonic delay line memory and spray velocity can adjust as the case may be, and described ultrasonic ultrasonic delay line memory also can multiplely be arranged in parallel.
In the present invention, described cyclone the tolerance etc. of absorption cleaning as required can select different size, or the parallel connection of multiple cyclone uses
In a second aspect of the present invention, provide a kind of device of ultrasonic atomizatio drop selective desulfurization hydrogen, this device comprises:
Ultrasonic ultrasonic delay line memory, for being atomized by methyl diethanolamine, drop is dispersed;
Droplet distribution pipe, wherein said ultrasonic ultrasonic delay line memory is placed on bottom in droplet distribution pipe, and sulfide hydrogen gaseous mixture entrained drip in droplet distribution pipe enters cyclone rapidly;
The cyclone be connected with droplet distribution pipe, gaseous mixture fully contacts in cyclone instantaneously with drop, synchronously completes the process of reaction, selective absorbing hydrogen sulfide and gas-liquid separation.
In the present invention, the top of cyclone is overfall, and the gaseous mixture after purification is discharged by the overfall of cyclone; The bottom of cyclone is underflow opening, and the reclaiming after the underflow opening enrichment of cyclone of isolated methyl diethanolamine amine liquid, recycles.
In the present invention, by methyl diethanolamine atomization evenly, size droplet diameter is no more than 50 microns to ultrasonic ultrasonic delay line memory, thus increases methyl diethanolamine and contact with hydrogen sulfide area, improves absorption efficiency, and shortens the reaction time.
In the present invention, the time that gas enters cyclone narrows down to the shortest, while guarantee absorbing hydrogen sulphide efficiency, avoids the haptoreaction of methyl diethanolamine and carbon dioxide substantially, and what enhance hydrogen sulfide absorption is selective.
In the present invention, methyl diethanolamine drop is brought into cyclone with reverse contact of gaseous mixture, the concentration≤10ppm of hydrogen sulfide in the gaseous mixture after desulfurization.
In the present invention, described gas entrained drip carries out gas-liquid separation rapidly in cyclone, and gas-liquid separation efficiency is not less than 90%.
In the present invention, described cyclone separator nominal manipulation pressure in normal conditions reduces to 0.00015-0.00025MPa.
Below referring to accompanying drawing.
Fig. 1 is the schematic flow sheet of the ultrasonic atomization drop selective desulfurization hydrogen technique of an embodiment according to the application.As shown in Figure 1, methyldiethanolamine solution atomization is drop by the ultrasonic ultrasonic delay line memory 1 being placed in bottom in droplet distribution pipe 2, drop and the sulfide hydrogen gaseous mixture Homogeneous phase mixing being entered droplet distribution pipe 2 by the entrance of droplet distribution pipe 2 of gained, and mixture is sprayed in cyclone 3 by the outlet of droplet distribution pipe 2, hydrogen sulfide in drop absorption gaseous mixture, purified gas is discharged from the overfall of cyclone 3, drop is separated in the eddy flow field of cyclone 3 simultaneously, the reclaiming after the underflow opening enrichment of cyclone of isolated methyl diethanolamine amine liquid (enriched amine liquid), recycle.
Major advantage of the present invention is:
(1) method of the present invention overcomes in existing gas sweetening hydrogen technical process and uses the desulfurizing tower such as plate column, packed tower equipment to cause methyl diethanolamine fully cannot contact with gas, substantially increases the problem of the loss of methyl diethanolamine and the energy charge of regeneration of absorption solution system.By methyl diethanolamine is become droplet morphology, in cyclone, rapid haptoreaction absorbs, and the rotating flow simultaneously carrying out solution-air is separated, and reduces methyl diethanolamine loss, alleviates regenerative system energy consumption, and improve the productivity ratio of downstream sulfur product.
(2) drop selective desulfurization hydrogen production device of the present invention, adopts cyclone to be key reaction separation equipment, compact conformation is simple, floor space is little, runs efficient stable, there is reaction speed fast, selective absorbing precision is high, and separative efficiency is high, the obvious advantage of the low grade of energy consumption.
(3) method and apparatus of ultrasonic atomizatio drop selective desulfurization hydrogen of the present invention, the methods such as the spray-absorption of conventional filler of comparing tower, methyl diethanolamine circulation consumption is less, and regeneration energy consumption reduces, and reduce equipment investment, society, economy and environmental benefit are remarkable.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment.But, should be understood that these embodiments only do not form limitation of the scope of the invention for illustration of the present invention.The test method of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.Except as otherwise noted, all percentage and number are by weight.
embodiment 1:
At a 50000m 3the natural gas of/h is produced in treatment process, according to method of the present invention, adopt drop reinforcing desulfuration decarbonization device, in order to carry out idetified separation to the natural gas gaseous mixture containing hydrogen sulfide and carbon dioxide etc., reach to complete with high efficiency, low-loss and be separated with the effective of sour gas the natural gas in multiple sour gas gaseous mixture, its concrete operation and effect are described below:
1. mist character and operating condition
Gaseous mixture is natural gas, and main component is 96% alkane, 1% hydrogen sulfide and about 9% carbon dioxide.Natural gas processing amount is 5000m 3/ h, density of gas phase operating temperature is 50 DEG C, and operating pressure is 2.7MPa.The concentration of N-Propylene Glycol amine aqueous solution (methyl diethanolamine) is 20-40%, is atomized by ultrasonic ultrasonic delay line memory, and average atomizing particle diameter is to less than 50 microns.
2. embodiment
Methyl diethanolamine drop is produced by ultrasonic ultrasonic delay line memory, and average droplet particles diameter is to less than 50 microns; The gaseous mixture of sulfur-bearing carbon containing enters cyclone rapidly; In cyclone, a large amount of methyl diethanolamine drop fully contacts with the sulphur carbon component in mist and reacts; Then, the gas after desulfurization and decarburization is entrained with methyl diethanolamine drop and enters cyclone, carries out the solution-air cyclonic separation of ultra low pressure drop; Be separated with the gaseous mixture after purification by methyl diethanolamine, pressure drop is less than 30mmH 2o(300Pa); In purified gas, the content of hydrogen sulfide is less than 10ppm; Methyl diethanolamine drop enriching and recovering regenerates, and recycles.
3. experimental result
After being separated by using drop reinforcing desulfuration decarbonization method, cyclone gaseous phase outlet hydrogen sulfide content is not more than 10ppm, carries liquid content secretly and is less than 50mg/m 3.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after having read above-mentioned instruction content of the present invention.

Claims (9)

1. a method for ultrasonic atomizatio drop selective desulfurization hydrogen, the method comprises the following steps:
I () utilizes ultrasonic atomization by methyldiethanolamine solution atomization for particle diameter is the drop of 10-50 μm;
(ii) the methyl diethanolamine drop of gained is mixed with hydrogen sulfide containing gas uniform, and within the time being no more than 1 second, mixture is sprayed in cyclone;
(iii) in cyclone, the hydrogen sulfide in methyl diethanolamine drop absorption gas, methyl diethanolamine drop is separated in the eddy flow field of cyclone simultaneously, and assembles the rich hydrogen sulfide containing methyl diethanolamine liquid of formation; And
(iv) after rich hydrogen sulfide containing methyl diethanolamine liquid regeneration, then it is atomized as drop by ultrasonic atomization, and the drop of gained is cycled to used in above-mentioned steps (ii),
Wherein, in cyclone, methyl diethanolamine drop and hydrogen sulfide containing gas carry out cyclonic separation simultaneously, and methyl diethanolamine drop is separated in the eddy flow field of cyclone, and separative efficiency is higher than 90%, and maximum pressure falls and is not more than 30mmH 2o.
2. the method for claim 1, is characterized in that, described hydrogen sulfide containing gas contains hydrogen sulfide and carbon dioxide, and wherein the concentration of hydrogen sulfide is between 100-10000ppm.
3. the method for claim 1, is characterized in that, in cyclone, hydrogen sulfide containing gas and the abundant haptoreaction of methyl diethanolamine drop, hydrogen sulfide is fully absorbed by methyl diethanolamine drop, and absorptivity is higher than 99.5%.
4., for a device for the method for the ultrasonic atomizatio drop selective desulfurization hydrogen any one of claim 1-3, this device comprises:
Ultrasonic ultrasonic delay line memory (1), for by methyldiethanolamine solution atomization for particle diameter is the drop of 10-50 μm;
In pipe, bottom arranges the droplet distribution pipe (2) of ultrasonic ultrasonic delay line memory (1), for being mixed with hydrogen sulfide containing gas uniform by the methyl diethanolamine drop of gained;
The cyclone (3) be connected with droplet distribution pipe (2), be provided for the hydrogen sulfide in methyl diethanolamine drop absorption gas, methyl diethanolamine drop is separated in the eddy flow field of cyclone simultaneously, and assemble the rich hydrogen sulfide containing methyl diethanolamine liquid of formation, wherein, separative efficiency is higher than 90%, and maximum pressure falls and is not more than 30mmH 2o.
5. device as claimed in claim 4, it is characterized in that, described droplet distribution pipe (2) is connected to gas feed, gas is entrained with methyl diethanolamine drop and enters in cyclone (3) in pipe, methyl diethanolamine drop fully contacts absorption with the hydrogen sulfide in gas, and in the gas after desulfurization, the concentration of hydrogen sulfide is less than 20ppm.
6. device as claimed in claim 4, it is characterized in that, the reaction of methyl diethanolamine drop absorption hydrogen sulfide is carried out under Elevated Gravity, and the haptoreaction time is less than 0.1 second.
7. device as claimed in claim 4, it is characterized in that, described cyclone (3) also carries out the gas-liquid separation of methyl diethanolamine drop and hydrogen sulfide gas simultaneously, purified gas is discharged from the overfall of cyclone (3), and drop enrichment enters amine liquid regenerating unit regeneration Posterior circle and utilizes.
8. device as claimed in claim 4, it is characterized in that, the quantity of described ultrasonic ultrasonic delay line memory (1) is one or more.
9. device as claimed in claim 4, it is characterized in that, the quantity of described cyclone (3) is one or more.
CN201210339435.XA 2012-09-13 2012-09-13 Method and device for selectively removing hydrogen sulfide by use of ultrasonically atomized liquid droplets Active CN102806001B (en)

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CN105854559B (en) * 2016-05-04 2020-09-04 山东源根化学技术研发有限公司 Papermaking white mud desulfurization device and desulfurization process
CN108057334A (en) * 2017-02-28 2018-05-22 中国矿业大学 A kind of method that chemical absorbing liquid ultrasonic atomizatio spray eliminates the CO in restricted clearance
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