CN107537301B - Jet-type absorption reactor - Google Patents
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Abstract
The invention relates to a jet type absorption reactor, belonging to the technical field of reactors for sulfur recovery. The jet type absorption reactor comprises a reaction tube, the bottom of the reaction tube is connected with a jet device, the bottom of the jet device is provided with a feed inlet, a residual liquid outlet is arranged on a connecting pipeline between the reaction tube and the jet device, the side wall of the reaction tube is respectively provided with a solid slurry outlet, a clear liquid outlet and a residual gas outlet, various types of fluids can flow out of the reactor conveniently, solid-liquid separation is realized when gas-liquid reaction occurs, the position of the solid slurry outlet is higher than that of the clear liquid outlet, and the top of the reaction tube is provided with a built-in temperature measuring tube. The invention solves the problems of insufficient gas-liquid contact, complex structure, unstable separation effect and easy blockage in the existing reactor, and has the characteristics of sufficient gas-liquid reaction, high hydrogen sulfide absorption rate and good separation effect.
Description
Technical Field
The invention relates to a jet type absorption reactor, belonging to the technical field of reactors for sulfur recovery.
Background
The wide application of fossil energy such as coal, oil and natural gas enables the development of modern economy at a high speed, but a large amount of hydrogen sulfide gas, H, is generated in the production processes of natural gas purification, oil refining, gas production and the like2S is not only toxic, but also corrosive in aerobic or damp heat conditions, so H2The existence of S can not only harm human health, but also corrode metal pipelines, burn out instruments and meters and the like, and especially in the processes of natural gas transportation and large-scale petroleum hydrofining, H2The presence of S increases the occurrence of H in petroleum pipelines2Possibility of S stress corrosion cracking, of oil, gasSafe mining and transportation are greatly affected. Therefore, how to handle H2The problem of S waste gas is receiving more and more attention.
Conventional H2The S treatment process mainly comprises a Claus method and a wet absorption method. Both of these methods treat the hydrocarbon containing H2The gas of S can reach higher purification degree, sulfur is recovered while desulfurization, but the biggest disadvantage is that hydrogen element in the gas is oxidized into water and wasted. In order to realize comprehensive utilization of resources, in recent years, H which can recover both sulfur and hydrogen has been developed2The new technology of S treatment, the indirect electrolysis method, is emphasized by people. The indirect electrolysis method is to oxidize H in the waste gas by using the absorption liquid2S, generating elemental sulfur, sending the reduced absorption liquid to the anode of the electrolytic cell for electrolytic regeneration and recycling, and generating hydrogen at the cathode of the electrolytic cell. The reaction system mainly comprises an absorption reactor and an electrolysis reactor, and H2The process of S absorption oxidation is generally carried out in an absorption reactor. Therefore, the design of the absorption reactor is particularly critical to the implementation of the whole process, in order to enable the gas to be in full contact with the absorption liquid to react, the prior art mostly adopts a bubbling mode to introduce the gas into the absorption liquid, and the structures of the absorption reactors are different due to different specific processes.
ZL200620004518.3 discloses a bubbling type absorption reactor, as shown in figure 2, in the using process of the reactor, because sulfur particles formed by gas-liquid reaction are fine or sticky and easily block a nozzle, the operation is intermittent in the currently applied process, continuous operation for efficiently absorbing hydrogen sulfide and simultaneously preparing hydrogen is difficult to realize, and research results show that gas-liquid contact is insufficient in the absorption operation, and the absorption rate of the hydrogen sulfide is not high.
ZL200620004518.3 discloses an internal circulation type absorption reactor, specifically, see fig. 3, which is improved in terms of improving the hydrogen sulfide absorption efficiency, preventing sulfur clogging and continuous operation, but when the reaction scale is enlarged, it is complicated to balance the load between the reaction units, and at the same time, the internal circulation type reactor is complicated in structure and high in manufacturing and maintenance costs.
In addition, the absorption reactor used for the technology of producing hydrogen and sulfur by electrolyzing hydrogen sulfide at present can not achieve the effect of solid-liquid separation, which can cause the problems of large filtering load and unstable separation effect in the process of filtering and separating sulfur and absorption liquid, and fine sulfur particles can possibly cause blockage in an electrolytic cell due to deposition in the long-time operation process.
Disclosure of Invention
The invention aims to provide a jet-type absorption reactor, which solves the problems of insufficient gas-liquid contact, complex structure, unstable separation effect and easy blockage in the existing reactor and has the characteristics of sufficient gas-liquid reaction, high hydrogen sulfide absorption rate and good separation effect.
The jet type absorption reactor comprises a reaction tube, wherein the bottom of the reaction tube is connected with a jet device, the bottom of the jet device is provided with a feed inlet, a residual liquid outlet is arranged on a connecting pipeline between the reaction tube and the jet device, the side wall of the reaction tube is respectively provided with a solid slurry outlet, a clear liquid outlet and a residual gas outlet, so that various types of fluids can flow out of the reactor conveniently, solid-liquid separation is realized while gas-liquid reaction is carried out, the position of the solid slurry outlet is higher than that of the clear liquid outlet, and the top of the reaction tube is provided with a built-in temperature measuring tube.
Wherein:
the connecting pipeline of the reaction tube and the ejector is a plastic tube, and the shorter the length of the plastic tube used as the connecting section is, the better the connecting section is.
The height-diameter ratio of the reaction tube is 9-11.
The tube wall of the temperature measuring tube and the tube wall of the reaction tube are in a sealed state, the upper end of the temperature measuring tube is open, the lower end of the temperature measuring tube is sealed, and the lower end of the temperature measuring tube keeps a certain distance from the bottom end of the reaction tube; whether a thermocouple needs to be inserted into the temperature measuring tube or not can be determined according to experimental conditions.
When the jet type absorption reactor is used, reaction gas and reaction liquid enter the reaction tube through the jet of the jet device, the gas is dispersed into fine bubbles under the carrying of the high-speed flowing liquid, the fine bubbles and the liquid ascend in the reaction tube together, and the gas and the liquid are fully contacted and mixed to react in the ascending process, so that the reaction efficiency is improved. In addition, gas and liquid can continuously generate solid products in the process of ascending in the reaction tube together, residual unreacted gas is attached to the surface of solid particles, the solid particles float up to the liquid level of the reaction liquid along with the gas under the driving of the jet power of the jet device and the automatic floating of the gas, and are led out through a solid slurry outlet at the upper part of the reaction tube, the liquid in the reaction tube becomes clear liquid due to the fact that most of the solid particles are separated by air floatation, the clear liquid can be led out from a clear liquid outlet at the middle part of the reaction tube, the load is lightened for subsequent filtering separation, the back flushing period of a filter can be greatly prolonged, and the filtering precision during high filtering flow is ensured.
The invention has the following beneficial effects:
(1) the jet type absorption reactor has dual functions of absorption and solid-liquid separation, is suitable for a process for generating solid after gas-liquid contact reaction, is beneficial to full contact of gas and liquid to improve the reaction efficiency, and can achieve the effect of solid-liquid separation, thereby avoiding the problems that solid particles generated by reaction block the jet device and are attached to the wall of the reactor, and reducing the load for subsequent solid filtering and separation;
(2) the ejector is positioned at the lower end of the reaction tube and is a necessary part for gas-liquid to meet and mix and enter the reaction tube, solid particles generated by gas-liquid reaction are not easy to deposit or attach to the tube wall in the ejector and the reaction tube due to the driving of high-flow-rate liquid, the blockage of the absorption reactor can be effectively avoided, and the gas-liquid contact area is also strengthened by the high dispersion of gas-liquid mixed flow.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the structure of a bubbling absorption reactor in comparative example 1;
FIG. 3 is a schematic view of the structure of an absorption reactor of internal circulation type in comparative example 2.
In the figure: 1. a temperature measuring tube; 2. a residual gas outlet; 3. a solid slurry outlet; 4. a clear liquid outlet; 5. a reaction tube; 6. an ejector; 7. a feed inlet; 8. and (5) residual liquid is led out.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
As shown in fig. 1, the jet type absorption reactor comprises a reaction tube 5, a jet device 6 is connected to the bottom of the reaction tube 5, a feed inlet 7 is arranged at the bottom of the jet device 6, a residual liquid outlet 8 is arranged on a connecting pipeline between the reaction tube 5 and the jet device 6, a solid slurry outlet 3, a clear liquid outlet 4 and a residual gas outlet 2 are respectively arranged on the side wall of the reaction tube, so that various types of fluids can flow out of the reactor respectively, solid-liquid separation is realized while gas-liquid reaction is carried out, the position of the solid slurry outlet 3 is higher than that of the clear liquid outlet 4, and a built-in temperature measuring tube 1 is arranged at the top of the reaction tube 5. Wherein, the connecting pipeline of the reaction tube 5 and the ejector 6 is a plastic tube, the height-diameter ratio of the reaction tube 5 is 9-11, and the tube wall of the temperature measuring tube 1 and the tube wall of the reaction tube 5 are in a sealed state; the upper end of the temperature measuring tube 1 is open, the lower end is sealed, and the lower end keeps a certain distance from the bottom end of the reaction tube 5.
Example 2
Taking the treatment process of electrolyzing hydrogen sulfide to produce hydrogen and sulfur as an example, the absorption liquid used in the treatment process of electrolyzing hydrogen sulfide to produce hydrogen and sulfur is rich in Fe3+Fe (b) of3+/Fe2+Acid solution, the gas taking part in the reaction is H2And S. The jet type absorption reactor has the following specific working process:
H2S、N2and other component gases (e.g. ammonia, olefins, CO)2Etc.) are precisely distributed and metered by a three-way gas distribution device to be mixed into H-containing gas2S, wherein the volume content of hydrogen sulfide is 10-99%, the flow rate of the mixed gas is controlled by a gas flowmeter, and the mixed gas is rich in Fe3+The absorption liquid is mixed and then is fed into the reaction tube 5 at the feed inlet 7 under the injection action of the ejector 6, wherein the liquid-gas volume ratio is 5-20, and the total flow of the gas and the liquid is measured by a liquid flow meter. When the gas and the liquid pass through the jet device 6, the gas is dispersed into fine bubbles under the drive of the high-flow-rate liquid, and the bubbles freely rise in the absorption reaction pipe 5 and are absorbed simultaneouslyThe liquor undergoes the following reaction to produce sulphur: h2S+2Fe3+＝2H++2Fe2++ S ↓, sulfur which accounts for about 60-90 wt% of the total sulfur amount floats up to the liquid surface under the action of the jet power of the ejector 6 and the air bubbles to realize solid-liquid separation, and is led out through the solid slurry outlet 3 at the upper part of the reaction tube 5 in the form of slurry, the liquid in the reaction tube 5 becomes clear liquid due to the air-float separation of most sulfur particles, the clear liquid is led out from the clear liquid outlet 4 at the upper part of the reaction tube 5, and the unreacted gas enters the tail gas recovery pipeline through the residual gas outlet 2 and is sent to the alcohol amine absorption device. When the reactor is stopped, the residual liquid in the reaction tube 5 is led out from a residual liquid outlet 8 at the bottom of the reaction tube.
Compared with the reactor provided by the prior art, in the using process of the reactor, when gas and liquid pass through the ejector, the gas is dispersed into fine bubbles and reacts with the liquid in an ascending way, so that the gas-liquid contact area is increased, and the absorption efficiency is effectively improved; meanwhile, the generated sulfur is separated by air flotation, so that the phenomenon that sulfur particles block an absorption reactor is avoided, the load is reduced for subsequent sulfur filtration and separation, and the filtration precision is improved.
Example 3
The operation of the jet-flow type absorption reactor of this example was the same as that of example 2 except that H was measured under different reaction conditions2S absorption rate.
(1) H at different liquid/gas volume ratios2S absorption rate:
the absorption reaction pressure is normal pressure, the temperature is normal temperature, and Fe in the absorption liquid3+Concentration of about 0.6mol/L, Fe2+Concentration of about 0.2mol/L, H2SO4The hydrogen ion concentration of the system was 8 mol/L. According to the working range of the actual gas flowmeter, H2The flow rate of the mixed gas containing 60% by volume of S was fixed at 50L/h, and the liquid flow rate was varied to control the liquid/gas volume ratios at 6, 8, 10, 12 and 15, respectively. Respectively recording H in the acid gas entering the jet-type absorption reactor and the tail gas discharged from the jet-type absorption reactor2S content to calculate H2The absorption rate of S.
The results show that H2Of SThe absorption rates were all above 95%, and the absorption rates increased with increasing liquid/gas volume ratio, with the highest absorption rate in this test reaching above 99%. However, too large a liquid/gas volume ratio will affect H2The absorption rate of S, and therefore the liquid/gas volume ratio was chosen to be 10.
(2) H at different gas/liquid flow rates2S absorption rate:
the absorption reaction pressure is normal pressure, the temperature is normal temperature, and Fe in the absorption liquid3+Concentration of 0.6mol/L, Fe2+Concentration of 0.2mol/L, H2SO4The hydrogen ion concentration of the system was 8 mol/L. The ratio of liquid/gas was fixed at 10, the flow rates of gas and liquid were varied, and the pair H was measured2Influence of S absorption rate.
The results show that with increasing gas and liquid flow rates, H2The absorption rate of S gradually increases, while H2The S absorption rate gradually decreases due to the short gas-liquid contact time at high flow rates.
(3) Different H in the mixed gas2H at S content2S absorption rate:
the absorption reaction pressure is normal pressure, the temperature is normal temperature, and Fe in the absorption liquid3+Concentration of 0.6mol/L, Fe2+Concentration of 0.2mol/L, H2SO4The hydrogen ion concentration of the system was 8 mol/L. The flow rates of the stationary gas and liquid were 50L/h and 500L/h, respectively, i.e., the stationary liquid/gas volume ratio was 10. Changing H in mixed gas2The content of S is examined and H in the mixed gas is examined2The S volume contents of 10%, 30%, 60% and 95% respectively, and the other component gas is nitrogen.
Experiments show that H2H when the S volume content is 10%, 30%, 60% and 95% respectively2The absorptance of S was 99%, 97%, 95% and 95%, respectively. Illustrating the applicability of the absorption reactor of the invention to H2The mixed gas with a large variation range of S content. Therefore, if processing H2When the content of S in the mixed gas is low, the enrichment treatment is not needed in advance.
Comparative example 1
This comparative example, which used a bubble absorption reactor, as shown in figure 2,during working, firstly, the absorption liquid is added into the reaction tube from the liquid inlet, and then H-containing gas is introduced into the reaction tube through the nozzle2The gas of S contacts with the absorption liquid at the lower part of the reaction tube and reacts to generate sulfur. The liquid and sulfur after reaction are discharged from a bottom outlet, and the redundant tail gas is discharged from the upper part of the reactor.
The bubbling type absorption reactor was operated under the same reaction conditions as in the third case of example 3, i.e., normal temperature and pressure, and Fe in the absorption liquid3+Concentration of 0.6mol/L, Fe2+Concentration of 0.2mol/L, H2SO4The hydrogen ion concentration in the system is 8mol/L, and the flow rates of the fixed gas and the liquid are respectively 50L/h and 500L/h. H in the mixed gas2H is measured when the volume content of S is respectively 10%, 30%, 60% and 95%2The absorptance of S was 87%, 80%, 68% and 60%, respectively. This absorption effect is far less than the present invention.
In addition, the gas and liquid in the bubbling type absorption reactor in the comparative example contact at the lower end of the nozzle to react rapidly, the generated sulfur is gathered at the lower end, the phenomenon that the gas nozzle is blocked by sulfur particles can occur in long-time operation, and the gas nozzle needs to be cleaned at any time, so the current operation is intermittent.
In the working process of the invention, the gas and the liquid contact and react at the ejector, and the generated sulfur particles are not easy to deposit in the ejector and the reaction tube due to the driving of the high-flow-rate liquid, thereby effectively avoiding the blockage of the absorption reactor. In addition, the gas-liquid contact area is also strengthened by the high dispersion of the gas-liquid after passing through the jet device, which is beneficial to improving H2S absorption rate.
Comparative example 2
The comparative example used an internal circulation type absorption reactor, which, as shown in fig. 3, consisted of a nozzle and a reaction tube, the nozzle consisted of an inner tube and a sleeve, the sleeve was sleeved outside the inner tube, the upper part of the sleeve was closed with the outer wall of the inner tube, the lower part was connected to the outside, an annular gap was formed between the sleeve and the inner tube, and the side wall of the sleeve was also provided with a gas inlet communicating with the annular gap, the nozzle was inserted into the reaction tube from the upper part of the reaction tube; an inner conduit with two ports communicated with the reaction tube is sleeved in the reaction tube, and an interlayer is formed between the inner conduit and the reaction tube; during operation, gas enters from the gas inlet, absorption liquid enters from the liquid inlet, the gas is carried by the absorption liquid to enter the inner guide pipe of the reactor through the annular space of the nozzle, and returns from the interlayer after descending along the inner wall of the inner guide pipe, so that circulation is realized in the reactor, full contact of the gas and the liquid is facilitated, the reaction efficiency is improved, and meanwhile, the effect of preventing solid particles generated by reaction from blocking the gas nozzle can be achieved. However, the absorption reactor has a complicated structure and is expensive to manufacture and maintain. And it is not easy to balance the load between the reaction units when the reaction scale is enlarged.
An internal circulation type absorption reactor was operated under the same reaction conditions as in the third case of example 3, i.e., normal temperature and pressure, and Fe in the absorption liquid3+Concentration of 0.6mol/L, Fe2+Concentration of 0.2mol/L, H2SO4The hydrogen ion concentration in the system is 8mol/L, and the flow rates of the fixed gas and the liquid are respectively 50L/h and 500L/h. H in the mixed gas2H is measured when the volume content of S is respectively 10%, 30%, 60% and 95%2The absorptance of S was 99%, 95%, 90% and 89%, respectively. The absorption effect is not as good as the present invention.
The invention has the same advantages as the above, and also has the functions of simple structure and solid-liquid separation, thereby greatly reducing the use cost.
Claims (1)
1. The application of a jet-type absorption reactor in the technology of producing hydrogen and sulfur by electrolyzing hydrogen sulfide indirectly is characterized in that: the jet type absorption reactor comprises a reaction tube (5), the bottom of the reaction tube (5) is connected with a jet device (6), the bottom of the jet device (6) is provided with a feed inlet (7), a residual liquid outlet (8) is arranged on a connecting pipeline of the reaction tube (5) and the jet device (6), the side wall of the reaction tube is respectively provided with a solid slurry outlet (3), a clear liquid outlet (4) and a residual gas outlet (2), the position of the solid slurry outlet (3) is higher than that of the clear liquid outlet (4), and the top of the reaction tube (5) is provided with a built-in temperature measuring tube (1);
the connecting pipeline of the reaction tube (5) and the ejector (6) is a plastic tube;
the height-diameter ratio of the reaction tube (5) is 9-11;
the pipe wall of the temperature measuring pipe (1) and the pipe wall of the reaction pipe (5) are in a sealed state, and the upper end of the temperature measuring pipe (1) is open and the lower end is sealed;
the jet type absorption reactor has the following specific working process: the absorption liquid in the jet-flow type absorption reactor is rich in Fe3+Fe (b) of3+/Fe2+Acid solution, the gas participating in the reaction is hydrogen sulfide mixed gas, wherein the volume content of the hydrogen sulfide is 10-99%, the flow rate of the mixed gas is controlled by a gas flowmeter, and the mixed gas is rich in Fe3+The absorption liquid is mixed and then is sent into a reaction tube (5) at a feed inlet (7) under the injection action of an ejector (6), wherein the liquid-gas volume ratio is 5-20; when gas and liquid pass through the ejector (6), gas is dispersed into fine bubbles under the drive of high-flow-rate liquid, the bubbles rise freely in the absorption reaction pipe (5) and react with absorption liquid to generate sulfur, the sulfur floats up to the liquid level under the action of the injection power of the ejector (6) and the bubbles to realize solid-liquid separation, and is led out through a solid slurry outlet (3) at the upper part of the reaction pipe (5) in a slurry form, the liquid in the reaction pipe (5) becomes clear liquid due to air flotation separation of most sulfur particles, the clear liquid is led out from a clear liquid outlet (4) at the middle upper part of the reaction pipe (5), unreacted gas enters a tail gas recovery pipeline through a residual gas outlet (2) and is sent to an alcohol amine absorption device, and when the device stops, residual liquid in the reaction pipe (5) is led out through a residual liquid outlet (8) at the bottom of the reaction pipe.
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| CN202893516U (en) * | 2012-11-16 | 2013-04-24 | 安徽理工大学 | Spraying stirring air-absorption mixture type flotation machine |
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| CN205253375U (en) * | 2015-10-19 | 2016-05-25 | 中国矿业大学 | Column type flotation equipment |
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| JP2007029781A (en) * | 2005-07-22 | 2007-02-08 | Mitsubishi Heavy Ind Ltd | Wet oxidation apparatus and method for organic waste liquid |
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| CN202893516U (en) * | 2012-11-16 | 2013-04-24 | 安徽理工大学 | Spraying stirring air-absorption mixture type flotation machine |
| US20150321123A1 (en) * | 2014-05-08 | 2015-11-12 | Alstom Technology Ltd | Antifoam device and method of use for seawater foam control |
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