CN217757342U - Device for desulfurizing and deodorizing coal tar - Google Patents
Device for desulfurizing and deodorizing coal tar Download PDFInfo
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- CN217757342U CN217757342U CN202221686417.4U CN202221686417U CN217757342U CN 217757342 U CN217757342 U CN 217757342U CN 202221686417 U CN202221686417 U CN 202221686417U CN 217757342 U CN217757342 U CN 217757342U
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Abstract
The utility model discloses a device of peculiar smell is removed in desulfurization of coal-based tar, the device includes the flash column, the flash column board, flash column gas distributor, coal-based tar pump, alkali wash the blender in advance, alkali wash the jar in advance, alkali wash the pump in advance, one-level desulfurization liquid film contactor, one-level liquid film contactor inner core, one-level liquid film desulfurization knockout drum, second grade desulfurization liquid film contactor, second grade liquid film contactor inner core, second grade liquid film desulfurization knockout drum, dealkalization coalescence separator, the coalescence filter core, the doctor solution heater, the doctor solution regenerator, the demister, filler, regenerator column gas distributor, the doctor solution cooler, the doctor solution pump, fresh doctor solution jar, fresh doctor solution measuring pump. The device can realize the purpose of desulfurization and peculiar smell removal of coal tar, and simultaneously reduce the emission of desulfurization waste liquid.
Description
Technical Field
The utility model relates to a coal system tar desulfurization removes peculiar smell technical field, particularly, relates to a coal system tar desulfurization removes device of peculiar smell.
Background
China's coal reserves account for about 45% of the world's total reserves and are the first place in the world. At present, the coal reserves in the world can be used for about 200 years, the coal reserves in China can be used for about 500 years, and the oil and natural gas resources which are proved at present can only be used for about 50 years. The comprehensive utilization of coal includes several aspects of using coal as primary energy source, producing secondary energy source and chemical raw material by using coal. Along with economic development, coal is processed into clean and efficient secondary energy, and chemical raw materials such as oil, methanol fuel and the like are produced by using the coal, so that the utilization rate and the additional value of the coal can be greatly improved, and the development of the coal chemical industry is more and more emphasized by people.
Since the content of sulfides in coal is mostly about 1%, a certain amount of sulfides, mainly hydrogen sulfide and organic sulfur, are inevitably carried in coal products. The hydrogen sulfide, low molecular mercaptan, carbonyl sulfide, carbon disulfide and other sulfides in the coal tar are low in boiling point and quick in volatilization, so that the coal tar is easy to cause foul smell during loading and unloading, and the surrounding environment and the physical and psychological health of nearby people are seriously affected.
According to sampling analysis, the total sulfur of the coal tar is generally about 10000 mug/g and can be higher than 40000 mug/g, and the category and the proportion of sulfides in the coal tar are shown in the following table:
| name of sulfur form | Boiling point (. Degree.C.) | Ratio (%) |
| Hydrogen sulfide | -60.4 | 1-3 |
| Carbonyl sulfide | -50 | 0.1-0.3 |
| Methyl mercaptan | 6 | 20-40 |
| Ethanethiol | 36.2 | 10-20 |
| Dimethyl sulfide | 37.3 | 0.05-1 |
| Carbon disulfide | 46.5 | 0.05-0.1 |
| Isopropyl mercaptan | 52.6 | 0.5-5 |
| Propanethiol | 67-68 | 0.3-3 |
| Tert-butyl mercaptan | 62-67 | 0.5-1 |
| Isobutyl mercaptan | 88 | 0.5-1 |
| Thiophene(s) | 84.2 | 5-15 |
| Diethyl sulfide | 92-93 | 0.05-0.1 |
| N-butylmercaptan | 98.4 | 0.03-0.06 |
| Dimethyl disulfide | 109.6 | 0.1-0.3 |
| Methyl Ethyl disulfide | 137 | 1-5 |
| Diethyl disulfide | 152 | 0.01-0.02 |
| Other higher boiling point forms of sulfur | - | 30-60 |
The hydrodesulfurization technology is a very thorough oil product desulfurization technology, can convert the sulfur in various forms into hydrogen sulfide, and then removes the hydrogen sulfide by using a steam stripping method or an amine liquid extraction method, but the hydrogenation process has large investment on equipment and higher hydrogenation cost, and has poor economy for small-scale treatment amount of coal-made tar.
The coal tar is only a small byproduct of coal chemical enterprises, and is generally sold to downstream enterprises as chemical raw materials, and the downstream enterprises can determine whether to carry out raw material treatment according to the processing amount and process requirements of the coal tar of the enterprises, and adopt a technology with better economy to carry out the raw material treatment. However, since the total sulfur content of the coal tar is high, especially the volatile sulfur content in the low-boiling-point form, the foul smell caused by the coal tar during loading and unloading needs to be treated to reduce the influence on the surrounding environment, and is also beneficial to the sale, processing and utilization of the coal tar.
According to the physicochemical property characteristics of volatile low-boiling-point form sulfur (mainly aiming at sulfides with the boiling point lower than 70 ℃) in the coal tar, the technology adopts flash evaporation and nitrogen stripping to remove most of hydrogen sulfide in the coal tar so as to reduce the consumption of the hydrogen sulfide on subsequent pre-alkali washing alkali liquor; then, removing hydrogen sulfide by adopting a mixer for pre-alkali washing so as to reduce the consumption of residual hydrogen sulfide on the subsequent liquid membrane contactor extraction desulfurization liquid and the influence of hydrogen sulfide on the desulfurization effect; extracting the coal tar after hydrogen sulfide removal by adopting a liquid film contactor desulfurization solution, wherein a hydrolysis catalyst in the desulfurization solution can hydrolyze carbonyl sulfide and carbon disulfide in the coal tar to convert hydrogen sulfide and carbon dioxide, sodium hydroxide in the desulfurization solution can react with hydrogen sulfide to generate sodium sulfide, and the sodium hydroxide can also react with C4 low molecular mercaptan in the coal tar to generate sodium mercaptide, wherein the process comprises a plurality of chemical reactions and removal of the carbonyl sulfide, the carbon disulfide and the mercaptan; under the action of catalysts such as sulfonated cobalt phthalocyanine and the like, desulfurized rich desulfurization solution enters a filler oxidation tower and is blown into air for oxidation regeneration, sodium sulfide in the desulfurization solution reacts with oxygen to generate sodium thiosulfate and sodium sulfate, sodium mercaptan is oxidized to generate sodium hydroxide and disulfide, the sodium hydroxide is dissolved in the desulfurization solution and is circularly used for desulfurization of coal tar, the boiling point of the disulfide is above 109 ℃, the odor threshold value is only below one tenth of that of the mercaptan, and when the desulfurization solution is circularly used for desulfurization of the coal tar, the disulfide is dissolved in the coal tar, so that the mercaptan removal process is actually a process of converting the mercaptan into the disulfide, the sulfur is not actually removed, and only the odor is greatly reduced.
The mixer is characterized by a reaction formula of pre-alkali washing and hydrogen sulfide removal:
H 2 S + 2NaOH → Na 2 S + H 2 O
the following reactions exist in the desulfurization process of the liquid membrane contactor desulfurization solution:
COS + H 2 o (in the presence of a hydrolysis catalyst) → H 2 S + CO 2
CS 2 + 2H 2 O (in the presence of a hydrolysis catalyst) → 2H 2 S + CO 2
H 2 S + 2NaOH → Na 2 S + H 2 O
CO 2 + 2NaOH → Na 2 CO 3 + H 2 O
RSH + NaOH → NaSR + H 2 O
Under the conditions of certain temperature and pressure, a trace amount of catalysts such as sulfonated cobalt phthalocyanine and the like are dissolved in the desulfurization solution, the desulfurized rich desulfurization solution enters a filler oxidation tower, air is blown into the tower through a gas distributor, and the following reactions occur in the oxidation regeneration process of the desulfurization solution:
2NaSR + 1/2 O 2 + H 2 O → 2NaOH + RSSR
2Na 2 S + 2O 2 + H 2 O → Na 2 S 2 O 3 + 2NaOH
Na 2 S 2 O 3 + 2O 2 + 2NaOH → 2Na 2 SO 4 + H 2 O
as can be seen from the above reaction formula, the sodium mercaptide produced by removing mercaptan can be completely oxidized to produce sodium hydroxide, while the sodium sulfide produced by removing hydrogen sulfide is finally converted into sodium thiosulfate and sodium sulfate. Therefore, the loss of the sodium hydroxide in the pre-alkaline washing alkali liquor and the desulfurization liquid by the hydrogen sulfide is permanent, the hydrogen sulfide in the coal tar is removed as much as possible in the flash evaporation and nitrogen stripping processes, and the hydrogen sulfide in the coal tar after the pre-alkaline washing is controlled to be completely removed.
SUMMERY OF THE UTILITY MODEL
In order to achieve the technical purpose, the technical scheme of the utility model is realized as follows:
a device for desulfurizing and deodorizing coal tar comprises a flash tower, wherein a flash tower plate is arranged in the flash tower, a flash tower gas distributor is arranged at the lower part of the flash tower, a coal tar inlet at the upper part of the flash tower is connected with a coal tar raw material pipe, a nitrogen inlet at the lower part of the flash tower is connected with a nitrogen pipe, the nitrogen inlet of the flash tower is connected with the flash tower gas distributor, a tail gas outlet at the top of the flash tower is connected with a flash tail gas pipe, a coal tar outlet at the bottom of the flash tower is connected with a coal tar pipe after flash evaporation, a coal tar oil pipe after flash evaporation is also connected with a pre-alkali washing mixer and a coal tar alkali liquor inlet at the top of a pre-alkali washing tank, a coal tar outlet at the other side of the top of the pre-alkali washing tank is connected with a coal tar pipe after hydrogen sulfide removal, an alkali liquor outlet at the bottom of the pre-alkali washing tank is connected with a pre-alkali washing alkali liquor pipe, the alkali washing alkali liquor pipe is also connected with a pre-alkali washing pump and a pre-alkali washing mixer inlet, the other end of the coal coking oil pipe after hydrogen sulfide removal is connected with a coal tar inlet at the top of a primary desulfurization liquid film contactor, a desulfurization liquid inlet at the top side of the primary desulfurization liquid film contactor is connected with a regeneration desulfurization liquid pipe II, the primary desulfurization liquid film contactor is mounted on a primary liquid film desulfurization separation tank through a flange, a desulfurization liquid outlet at the bottom of the primary liquid film desulfurization separation tank is connected with a desulfurization rich liquid pipe, a coal tar outlet at the other side of the top of the primary liquid film desulfurization separation tank is connected with a coal tar pipe after primary desulfurization, the other end of the coal tar pipe after primary desulfurization is connected with a coal tar inlet at the top of a secondary desulfurization liquid film contactor, a desulfurization liquid inlet at the top side of the secondary liquid film contactor is connected with a regeneration desulfurization liquid pipe I, and the secondary desulfurization contactor is mounted on a secondary desulfurization liquid film separation tank through a flange, the desulfurization separation tank of second grade liquid film desulfurization tank bottom doctor solution exit linkage rich desulfurization liquid pipe one, coal system tar oil pipe after second grade desulfurization is connected to second grade liquid film desulfurization separation tank top opposite side coal system tar exit linkage, second grade desulfurization back coal system tar pipe other end connects dealkalization coalescence separator coal system tar import, alkali coalescence separator top opposite side coal system tar exit linkage refined coal system tar oil pipe, dealkalization coalescence separator bottom part liquid package doctor solution exit linkage rich desulfurization liquid pipe two, rich desulfurization liquid pipe one is connected to two other ends of rich desulfurization liquid pipe, rich desulfurization liquid pipe is connected to one other end of rich desulfurization liquid pipe, rich desulfurization liquid pipe still is connected with doctor solution heater and doctor solution regeneration tower upper portion doctor solution pipe import, rich desulfurization liquid pipe still is connected with fresh doctor solution pipe, fresh doctor solution pipe still is connected with fresh desulfurizing liquid tank and fresh doctor solution, doctor solution regeneration tower lower part air inlet connects compressed air pipe, doctor solution regeneration tower upper portion inlet connects compressed air pipe, doctor solution regeneration tower top nitrogen gas outlet connection doctor solution regeneration tower top tail gas pipe, doctor solution regeneration tower tail gas outlet connection regeneration liquid regeneration one, doctor solution regeneration liquid regeneration outlet connection second doctor solution regeneration outlet still is connected with the doctor solution.
Furthermore, a first-stage liquid film contactor inner core and a second-stage liquid film contactor inner core are respectively arranged in the first-stage desulfurization liquid film contactor and the second-stage desulfurization liquid film contactor.
Furthermore, a coalescing filter element is arranged in the dealkalizing coalescing separator.
Furthermore, a demister is arranged at the top of the desulfurization liquid regeneration tower, a filler is arranged at the middle section of the desulfurization liquid regeneration tower, and a regeneration tower gas distributor is arranged at the lower part of the desulfurization liquid regeneration tower.
Further, 10 layers of flash tower plates are arranged in the flash tower, and the distance between adjacent flash tower plates is 400-800mm.
Furthermore, the first-stage desulfurization liquid film contactor and the second-stage desulfurization liquid film contactor respectively comprise a contactor shell, a contactor pore plate, fiber bundle lifting hooks and a contactor fiber bundle, each bundle of contactor fiber bundle corresponds to one fiber bundle lifting hook and one fiber bundle lifting hole, a plurality of fiber bundle lifting hooks on one straight line are fixed on the contactor pore plate through a fiber bundle lifting hook transverse pin, the fiber bundle lifting holes on the contactor pore plate are uniformly distributed, the length of the contactor fiber bundle is 2-10m, the contactor fiber bundle is composed of a large number of fibers with the diameter of 0.2-2.0mm, the surfaces of the fibers are subjected to chemical modification treatment, the fibers are in a continuous corrugated shape, the height of corrugations is 2-10mm, and the width of single-stage corrugations is 5-30mm.
Furthermore, the flash tower gas distributor and the regeneration tower gas distributor are both multi-row round tubes or square tubes which are uniformly perforated.
The utility model has the advantages that: the device for desulfurizing and deodorizing coal tar of the utility model adopts flash evaporation and nitrogen gas stripping to remove most hydrogen sulfide in coal tar, so as to reduce the consumption of hydrogen sulfide on the subsequent alkali washing alkali liquor; then, removing hydrogen sulfide by adopting a mixer for pre-alkali washing so as to reduce the consumption of residual hydrogen sulfide on the subsequent liquid membrane contactor extraction desulfurization liquid and the influence of hydrogen sulfide on the desulfurization effect; extracting the coal tar after hydrogen sulfide removal by adopting a liquid film contactor desulfurization solution, hydrolyzing carbonyl sulfide and carbon disulfide in the coal tar by using a hydrolysis catalyst in the desulfurization solution to convert the carbonyl sulfide and the carbon disulfide into hydrogen sulfide and carbon dioxide, reacting sodium hydroxide in the desulfurization solution with hydrogen sulfide to generate sodium sulfide, and reacting the sodium hydroxide with volatile low-molecular mercaptan with the boiling point of below 70 ℃ in the coal tar to generate sodium mercaptide; a trace amount of catalysts such as sulfonated cobalt phthalocyanine and the like are also dissolved in the desulfurization solution, the desulfurized rich desulfurization solution enters a filler oxidation tower, air is blown into the filler oxidation tower, sodium sulfide in the desulfurization solution reacts with oxygen to generate sodium thiosulfate and sodium sulfate, sodium mercaptan is oxidized to generate sodium hydroxide and disulfide, the sodium hydroxide is dissolved in the desulfurization solution and is circularly used for desulfurization of coal tar, the boiling point of the disulfide is above 109 ℃, the odor threshold value is only below one tenth of that of the mercaptan, when the desulfurization solution is circularly used for desulfurization of the coal tar, the disulfide is dissolved in the coal tar, and hydrogen sulfide, carbonyl sulfide and carbon disulfide in the coal tar are removed, so that the purposes of desulfurization and odor removal of the coal tar are achieved.
The combined process of flash evaporation, nitrogen stripping, mixer pre-alkali washing to remove hydrogen sulfide, liquid membrane contactor to remove carbonyl sulfide, carbon disulfide and low molecular weight mercaptan, dealkalization coalescence separator to remove free desulfurization liquid and rich desulfurization liquid to catalyze air oxidation regeneration is adopted, hydrogen sulfide in coal tar can be completely removed, the removal rate of carbonyl sulfide and carbon disulfide can reach more than 90%, the removal rate of methyl mercaptan can reach more than 99%, the removal rate of ethyl mercaptan can reach more than 95%, the removal rate of C3 mercaptan can reach more than 80%, the removal rate of C4 mercaptan can reach more than 60%, and the content of free desulfurization liquid carried in refined coal tar is not more than 10 microgram/g. Most of volatile hydrogen sulfide, carbonyl sulfide and carbon disulfide which have boiling points below 70 ℃ and easily cause foul smell in the coal tar are removed, and low-molecular mercaptan below C4 is converted into disulfide with relatively much lower odor threshold, so that the aims of desulfurization and odor removal of the coal tar are fulfilled, and the emission of desulfurization waste liquid can be greatly reduced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a device for desulfurizing and deodorizing coal tar according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a liquid membrane contactor of a device for desulfurizing and deodorizing coal tar according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a contactor orifice plate of the device for desulfurizing and deodorizing coal tar according to the embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a gas distributor of a flash tower and an alkali liquor regeneration tower of the device for desulfurizing and deodorizing coal tar according to the embodiment of the present invention;
in the figure: 1. a flash tower, 2, a flash tower plate, 3, a flash tower gas distributor, 4, a coal tar pump, 5, a pre-alkaline washing mixer, 6, a pre-alkaline washing tank, 7, a pre-alkaline washing pump, 8, a primary desulfurization liquid film contactor, 9, a primary liquid film contactor inner core, 10, a primary liquid film desulfurization separation tank, 11, a secondary desulfurization liquid film contactor, 12, a secondary liquid film contactor inner core, 13, a secondary liquid film desulfurization separation tank, 14, a dealkalization coalescence separator, 15, a coalescence filter element, 16, a desulfurization liquid heater, 17, a desulfurization liquid regenerator, 18, a demister, 19, a filler, 20, a regenerator tower gas distributor, 21, a desulfurization liquid cooler, 22, a desulfurization liquid pump, 23, a fresh desulfurization liquid tank, 24, a fresh desulfurization liquid metering pump, 31, a coal tar raw material pipe, 32, a coal coking oil pipe after flash evaporation, 33, a coal coking oil pipe after hydrogen sulfide removal, 34, a coal coking oil pipe after primary desulfurization, 35, a coal coking oil pipe after secondary desulfurization, 36, a refined coal coking oil pipe, 37, a nitrogen pipe, 38, a flash evaporation tail gas pipe, 40, a first regenerated desulfurization liquid pipe, 41, a second regenerated desulfurization liquid pipe, 43, a caustic soda washing liquid pipe, 44, a rich desulfurization liquid pipe, 45, a first rich desulfurization liquid pipe, 46, a second rich desulfurization liquid pipe, 47, a fresh desulfurization liquid pipe, 49, a compressed air pipe, 50, a compressed nitrogen pipe, 51, a regenerated desulfurization liquid tail gas pipe, 81, a contactor shell, 82, a contactor pore plate, 83, a fiber bundle hook, 84, a contactor fiber bundle, 85, a fiber bundle hanging hole, 86 and a fiber bundle hook transverse pin.
Detailed Description
The technical solutions in the embodiments of the present invention will be described below clearly and completely, and it should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art all belong to the protection scope of the present invention.
As shown in figures 1-4, according to the device for desulfurizing and deodorizing coal tar according to the embodiment of the present invention, the device comprises a flash tower 1, a flash tower plate 2 is arranged in the flash tower 1, a flash tower gas distributor 3 is arranged at the lower part of the flash tower 1, a coal tar inlet at the upper part of the flash tower 1 is connected with a coal tar raw material pipe 31, a nitrogen inlet at the lower part of the flash tower 1 is connected with a nitrogen pipe 37, a nitrogen inlet of the flash tower 1 is connected with the flash tower gas distributor 3, a tail gas outlet at the top of the flash tower 1 is connected with a flash tail gas pipe 38, a coal tar outlet at the bottom of the flash tower 1 is connected with a coal tar pipe 32 after flash evaporation, the coal tar pipe 32 after flash evaporation is further connected with a pre-alkali washing mixer 5 and a coal tar alkali liquid inlet at the top of the pre-alkali washing tank 6, a coal tar outlet at the other side of the top of the pre-alkali washing tank 6 is connected with a coal tar oil pipe 33 after hydrogen sulfide removal, the alkali liquor outlet at the bottom of the pre-alkali washing tank 6 is connected with a pre-alkali washing alkali liquor pipe 43, the pre-alkali washing alkali liquor pipe 43 is further connected with a pre-alkali washing pump 7 and a coal-made tar pipe 32 which is flash-evaporated at the inlet of a pre-alkali washing mixer 5, the other end of the coal-made tar pipe 33 after hydrogen sulfide removal is connected with a coal-made tar inlet at the top of a primary desulfurization liquid film contactor 8, the desulfurization liquid inlet at the top of the primary desulfurization liquid film contactor 8 is connected with a regeneration desulfurization liquid pipe II 41, the primary desulfurization liquid film contactor 8 is arranged on a primary liquid film desulfurization separation tank 10 through a flange, the desulfurization liquid outlet at the bottom of the primary liquid film desulfurization separation tank 10 is connected with a desulfurization-rich liquid pipe 44, the coal-made tar outlet at the other side of the top of the primary liquid film separation tank 10 is connected with a coal-made tar pipe 34 after primary desulfurization, the other end of the coal-made tar pipe 34 after primary desulfurization is connected with a coal-made tar inlet at the top of a secondary desulfurization liquid film contactor 11, second grade desulfurization liquid film contactor 11 top side doctor solution access connection regeneration desulfurization liquid pipe 40, second grade desulfurization liquid film contactor 11 passes through the flange mounting on second grade liquid film desulfurization knockout drum 13, second grade liquid film desulfurization knockout drum 13 bottom doctor solution exit linkage rich desulfurization liquid pipe 45, second grade liquid film desulfurization knockout drum 13 top opposite side coal system tar exit linkage second grade desulfurization back coal system tar pipe 35, dealkalization coalescence separator 14 coal system tar import is connected to second grade desulfurization back coal system tar pipe 35 other end, dealkalization coalescence separator 14 top opposite side coal system tar exit linkage refined coal system tar pipe 36, dealkalization coalescence separator 14 bottom partial liquid package doctor solution exit linkage rich desulfurization liquid pipe two 46, rich desulfurization liquid pipe two 46 other ends connect rich desulfurization liquid pipe 45, rich desulfurization liquid pipe 45 other end connection rich desulfurization liquid pipe 44, rich desulfurization liquid pipe 44 still is connected with doctor solution heater 16 and desulfurization liquid regeneration tower 17 upper portion doctor solution pipe import, rich desulfurization liquid pipe 44 still is connected with fresh desulfurization liquid 47, fresh desulfurization liquid pipe 47 still is connected with fresh desulfurization liquid tank 23 and desulfurization liquid compressed air regeneration tower 17, desulfurization liquid regeneration tower 17 regeneration tail gas regeneration tower inlet connection desulfurization liquid regeneration air regeneration tower 17, desulfurization liquid regeneration tower exit linkage 18, desulfurization liquid regeneration air regeneration tower regeneration liquid regeneration inlet 49, desulfurization liquid regeneration tower regeneration air regeneration nitrogen regeneration liquid regeneration tower 17, desulfurization liquid regeneration tower exit linkage.
The first-stage desulfurization liquid film contactor 8 and the second-stage desulfurization liquid film contactor 11 are internally provided with a first-stage liquid film contactor inner core 9 and a second-stage liquid film contactor inner core 12 respectively.
The dealkalizing coalescer 14 is provided with a coalescer element 15.
A demister 18 is arranged at the top of the desulfurization solution regeneration tower 17, a filler 19 is arranged at the middle section of the desulfurization solution regeneration tower 17, and a regeneration tower gas distributor 20 is arranged at the lower part of the desulfurization solution regeneration tower 17.
10 layers of flash tower plates 2 are arranged in the flash tower 1, and the distance between every two adjacent flash tower plates 2 is 400-800mm.
The first-stage desulfurized liquid film contactor 8 and the second-stage desulfurized liquid film contactor 11 respectively comprise a contactor shell 81, a contactor pore plate 82, fiber bundle hooks 83 and contactor fiber bundles 84, each bundle of contactor fiber bundles 84 corresponds to one fiber bundle hook and one fiber bundle hanging hole 85, a plurality of fiber bundle hooks on one straight line are fixed on the contactor pore plate 82 through one fiber bundle hook cross pin 86, the fiber bundle hanging holes 85 on the contactor pore plate 82 are uniformly distributed, the length of the contactor fiber bundles 84 is 2-10m, the contactor fiber bundles 84 are composed of a plurality of fiber filaments with the diameters of 0.2-2.0mm, the surfaces of the fiber filaments are subjected to chemical modification treatment, the fiber filaments are in a continuous corrugated shape, the height of the corrugations is 2-10mm, the width of the single-stage corrugations is 5-30mm, and the first-stage desulfurized liquid film contactor 8 and the second-stage desulfurized liquid film contactor 11 can be designed into one stage or multiple stages according to the low molecular form sulfur content and the requirements of desulfurization and odor removal in coal tar.
The flash tower gas distributor 3 and the regeneration tower gas distributor 20 are multi-row round tubes or square tubes which are uniformly perforated, and the bubbles are uniformly distributed on the cross section in the tower.
The method for desulfurizing and deodorizing coal tar by adopting the device for desulfurizing and deodorizing coal tar provided by the embodiment of the utility model comprises the following steps:
s1, enabling sulfur-containing malodorous coal tar with the temperature of 20-50 ℃ and the pressure of more than 0.3MPa (G) to enter a flash tower from an upper coal tar inlet, controlling the pressure of the flash tower to be about 0.05 MPa (G), controlling the liquid level to be below the lowest tower plate in the tower, enabling the coal tar to flow through a plurality of tower plates in the tower layer by layer from top to bottom, enabling compressed nitrogen to pass through the plurality of tower plates in the tower from a nitrogen inlet at the lower part of the tower and be uniformly distributed on the cross section of the tower through a gas distributor in the tower from bottom to top, enabling the nitrogen to fully contact with the coal tar, enabling most hydrogen sulfide in the coal tar to be subjected to pressure reduction and nitrogen stripping and mixed with the nitrogen to form valve steaming tail gas which is discharged from the top of the tower to a torch or an incinerator;
s2, performing flash evaporation and nitrogen stripping to remove most of hydrogen sulfide to obtain coal tar, pressurizing to 0.5-0.8 MPa (G) by using a coal tar pump, feeding the coal tar and the alkali solution to a pre-alkali washing layer mixer, reacting residual hydrogen sulfide and a small part of low-molecular mercaptan in the coal tar with sodium hydroxide in the alkali solution to generate sodium sulfide and sodium mercaptan, removing hydrogen sulfide in the coal tar to below 5 mu G/G, and when the content of hydrogen sulfide in the coal tar after the pre-alkali washing is close to about 5 mu G/G, intermittently replacing the alkali solution, wherein the initial concentration of the alkali solution is preferably 5-10 wt%;
s3, coal tar and circulating desulfurization liquid which are subjected to hydrogen sulfide pre-alkaline washing enter a desulfurization liquid film contactor from a coal tar inlet and a desulfurization liquid inlet respectively, the desulfurization liquid is a water phase, a water phase film is formed by extending the surfaces of hydrophilic fibers in the inner core of the liquid film contactor, the coal tar is dispersed into an oil phase film by countless fibers, the oil phase and the water phase are fully contacted in a liquid film mode and flow forward between the fibers in a laminar flow mode, carbonyl sulfide and carbon disulfide in the coal tar are hydrolyzed into hydrogen sulfide and carbon dioxide under the action of a hydrolysis catalyst in the desulfurization liquid, the hydrogen sulfide, the carbon dioxide and original low molecular mercaptan in the coal tar are fully contacted and reacted with sodium hydroxide in the desulfurization liquid, sodium sulfide, sodium carbonate and sodium mercaptide which are respectively generated are dissolved in alkali liquor, the coal tar after desulfurization is subjected to desulfurization by a dealkalization coalescence separator to remove the desulfurization solution which is carried in the coal tar, a one-stage or multi-stage desulfurization liquid film contactor is designed for desulfurization according to the contents of carbonyl sulfide, carbon disulfide and low molecular mercaptan in the coal tar, the removal rate of the carbonyl sulfide and the carbon disulfide in the coal tar can reach more than 90 percent in the process, the removal rate of methyl mercaptan can reach more than 99 percent, the removal rate of ethyl mercaptan can reach more than 95 percent, the removal rate of C3 mercaptan can reach more than 80 percent, the removal rate of C4 mercaptan can reach more than 60 percent, and the content of the free desulfurization solution carried in the refined coal tar does not exceed 10 microgrammes/gram;
s4, delivering desulfurized rich desulfurization liquid from a desulfurization liquid outlet at the bottom of a one-stage or multi-stage liquid film desulfurization separation tank under self pressure, heating the desulfurized rich desulfurization liquid to 40-50 ℃ through a desulfurization liquid heater, simultaneously connecting and supplementing fresh desulfurization liquid through a metering pump, feeding the desulfurized rich desulfurization liquid into a desulfurization liquid regeneration tower from a desulfurization liquid inlet at the upper part of the tower, wherein the middle section of the desulfurization liquid regeneration tower is provided with regular or scattered packing, the desulfurization liquid flows through the packing from top to bottom, compressed air enters from an air inlet at the lower part of the tower and is dispersed into fine bubbles through a gas distributor and uniformly distributed in the tower, the air bubbles flow through the packing from bottom to top, the desulfurization liquid and the air are respectively and continuously sheared when flowing through the packing, the two phases flow in opposite directions and are fully contacted, sodium sulfide in the desulfurization liquid reacts with oxygen in the bubbles to generate sodium thiosulfate and sodium sulfate under the action of catalysts such as sulfonated titanium phthalocyanine cobalt, and the like, sodium thiolate reacts with the oxygen in the bubbles to generate sodium hydroxide and disulfide, the generated sodium hydroxide is dissolved in the desulfurization solution for circularly desulfurizing the coal tar, a small part of the generated disulfide is taken away with tail gas, when most of the generated disulfide enters a desulfurization liquid membrane contactor along with the desulfurization solution, the generated disulfide enters the coal tar by back extraction, the disulfide has the boiling point of over 109 ℃ and the odor threshold value of less than one tenth of mercaptan, and hydrogen sulfide, carbonyl sulfide and carbon disulfide in the coal tar are removed, so that the aim of desulfurizing and deodorizing the coal tar is fulfilled through the processes, the removal of the hydrogen sulfide, the carbonyl sulfide and the carbon disulfide and the carbon dioxide in the air consume the sodium hydroxide in the desulfurization solution, therefore, the fresh desulfurization solution needs to be connected and supplemented, the concentration of the sodium hydroxide in the fresh desulfurization solution is preferably 20-25 wt%, and simultaneously, a corresponding amount of waste desulfurization solution is discharged, in order to avoid the formation of explosive gas by the tail gas containing the disulfide, at the same time, it is necessary to supplement the top of the desulfurization solution regeneration column with a flow rate of nitrogen gas such that the oxygen content in the desulfurization solution regeneration off-gas does not exceed 8% v.
The liquid-liquid ratio of the blown-off nitrogen gas to the coal tar gas in the S1 is in the range of 5-10, the temperature of the coal tar raw material is above 20 ℃, and the pressure drop of the coal tar after entering the flash tower is above 0.2 MPa.
The concentration of the pre-alkaline washing alkali liquor of the mixer in the S2 is in the range of 5-10%, and the mass flow of the circulating alkali liquor is 30-100% of the mass flow of the coal tar.
The mass flow of the desulfurization liquid entering the desulfurization liquid membrane contactor in the S3 is 20-60% of the mass flow of the coal tar.
The desulfurization solution in the S3 is prepared by compounding one or two of sodium hydroxide or potassium hydroxide, a hydrolysis catalyst, a cobalt phthalocyanine catalyst and water, wherein the concentration of the sodium hydroxide or the potassium hydroxide is in the range of 15-30%, the concentration of the hydrolysis catalyst is in the range of 10-30%, the concentration of the cobalt phthalocyanine catalyst is in the range of 100-200 mu g/g, the hydrolysis catalyst consists of an organic amine compound with the content of 50-80% by weight and a phase transfer catalyst with the content of 20-50% by weight, the organic amine compound consists of more than one primary amine compound, more than one tertiary amine compound and/or more than one secondary amine compound, and the primary amine compound is monoethanolamine and/or diglycolamine; the secondary amine compound is one or a mixture of diethanolamine, diisopropanolamine or N-methyl monoethanolamine; the tertiary amine compound is triethanolamine and/or N-methyldiethanolamine, the phase transfer catalyst is one or more of sulfolane, polyethylene glycol (200), polyethylene glycol (400), tetrabutylammonium bromide, tetrabutylammonium chloride, dodecyltrimethylammonium chloride, tetradecyltrimethylammonium chloride, pyridine or tributylamine, and the cobalt phthalocyanine catalyst is one or more of sulfonated cobalt phthalocyanine, poly cobalt phthalocyanine or ammonium cobalt phthalocyanine sulfonate.
The oxidation reaction of the rich desulfurization solution catalyzed by the rich desulfurization solution in the S4 is an exothermic reaction, the rich desulfurization solution is heated to a proper temperature by a heater, the operating temperature of a desulfurization solution regeneration tower is controlled within the range of 60-70 ℃, the operating pressure of the desulfurization solution regeneration tower is controlled within the range of 0.2-0.4MPa (G), the packing in the desulfurization solution regeneration tower is regular packing or random packing, and the material of the packing is stainless steel or an alkali-corrosion-resistant high polymer material.
For the convenience of understanding the above technical solutions of the present invention, the above technical solutions of the present invention are explained in detail through specific use modes below.
Example 1
A company provides a coal tar sample, total sulfur of the coal tar is 42875 mu g/g, wherein the content of hydrogen sulfide is 1257 mu g/g, the content of carbonyl sulfide is 924 mu g/g, the content of carbon disulfide is 38 mu g/g, the content of methyl mercaptan sulfur is 12755 mu g/g, the content of ethyl mercaptan sulfur is 5143 mu g/g, the content of C3 mercaptan is 439 mu g/g, the content of C4 mercaptan is 209 mu g/g, a flash tower nitrogen stripping and mixer is adopted to carry out pre-alkaline cleaning hydrogen sulfide, a three-stage liquid film contactor is adopted to carry out decarbonylation sulfur, carbon disulfide and low-molecular mercaptan, and a rich desulfurization liquid catalytic air oxidation regeneration combined process is adopted to carry out a desulfurization and odor removal pilot test experiment, hydrogen sulfide in refined coal tar is not detected, the content of carbonyl sulfide is 46 mu g/g, the content of carbon disulfide is 4.5 mu g/g, the content of methyl mercaptan is 18 mu g/g, the content of ethyl mercaptan sulfur is 191 mu g/g, the content of C3 mercaptan is 35 mu g/g, the content of C4 mercaptan is 73 mu g/g, and the odor of the coal tar is obviously reduced.
Example 2
According to the utility model, a set of desulfurization and odor removal device for coal tar is built by a company, the processing capacity of the coal tar is 5 tons/hour, the total sulfur of the coal tar is 12574 mu g/g, wherein, the hydrogen sulfide content is 329 mu g/g, the carbonyl sulfide content is 157 mu g/g, the carbon disulfide content is 98 mu g/g, the methyl mercaptan sulfur content is 4410 mu g/g, the ethanethiol sulfur content is 2782 mu g/g, the C3 mercaptan content is 628 mu g/g, and the C4 mercaptan content is 154 mu g/g, the hydrogen sulfide is pre-alkali-washed and dehydrated by a flash tower nitrogen blowing-off and mixer, the two-stage liquid film contactor desulfurization liquid is used for removing carbonyl sulfide, carbon disulfide and low molecular mercaptan, the dealkalization coalescence separator is used for removing free desulfurization liquid, and rich desulfurization liquid catalysis and air oxidation regeneration combined process, the hydrogen sulfide in the refined coal tar is not measured, the carbonyl sulfide content is 7.5 mu g/g, the carbon disulfide content is 12 mu g/g, the methyl mercaptan sulfur content is 17 mu g/g, the ethanethiol content is 84 mu g/g, the C3 mu g/g mercaptan content is 102 mu g, the free mercaptan content is about 1.8 mu g/g, and the odor of the free mercaptan is obviously reduced. About 1200 tons of waste alkali liquor is discharged in the process of pre-alkali washing every year, and about 100 tons of waste alkali liquor is discharged in the process of desulfurization.
Example 3
According to the utility model, a set of desulfurization and odor removal device for coal tar is built by a company, the processing capacity of the coal tar is 7 tons/hour, the total sulfur of the coal tar is 26142 mu g/g, wherein, the hydrogen sulfide content is 1017 mu g/g, the carbonyl sulfur content is 113 mu g/g, the carbon disulfide content is 72 mu g/g, the methyl mercaptan sulfur content is 9643 mu g/g, the ethyl mercaptan sulfur content is 6267 mu g/g, the C3 mercaptan content is 442 mu g/g, the C4 mercaptan content is 253 mu g/g, the hydrogen sulfide is pre-alkali-washed and desorbed by adopting a flash tower nitrogen blowing-off and mixer, the decarbonylation sulfur, the carbon disulfide and low-molecular mercaptan are desorbed by a three-level liquid membrane contactor desulfurizing liquid, the free desulfurizing liquid is desorbed by a dealkalization coalescence separator, and air oxidation regeneration combined process is catalyzed by the rich desulfurizing liquid, the hydrogen sulfide in the refined coal tar is not detected, the carbonyl sulfur content is 5.6 mu g/g, the carbon disulfide content is 2.8 mu g/g, the methyl mercaptan sulfur content is 15 mu g/241, the ethyl mercaptan content is 66 g, the C3 mu g/g, the free sulfur content is 97 mu g/g, the odor of the C3 g/g of the tar is obviously reduced, and the odor of the odor is reduced. About 1800 tons of waste alkali liquor is discharged in the process of pre-alkaline washing every year, and about 150 tons of waste alkali liquor is discharged in the process of desulfurization.
In conclusion, by means of the technical scheme of the utility model, most hydrogen sulfide in coal tar is removed by flash evaporation and nitrogen stripping, so as to reduce the consumption of hydrogen sulfide on the subsequent alkali washing liquid; then, removing hydrogen sulfide by adopting a mixer for pre-alkaline washing so as to reduce the consumption of residual hydrogen sulfide on the subsequent liquid membrane contactor extraction desulfurization liquid and the influence of hydrogen sulfide on the desulfurization effect; extracting the coal tar after hydrogen sulfide removal by adopting a liquid film contactor desulfurization solution, hydrolyzing carbonyl sulfide and carbon disulfide in the coal tar by using a hydrolysis catalyst in the desulfurization solution to convert the carbonyl sulfide and the carbon disulfide into hydrogen sulfide and carbon dioxide, reacting sodium hydroxide in the desulfurization solution with hydrogen sulfide to generate sodium sulfide, and reacting the sodium hydroxide with volatile low-molecular mercaptan with the boiling point of below 70 ℃ in the coal tar to generate sodium mercaptide; a trace amount of catalysts such as sulfonated cobalt phthalocyanine and the like are also dissolved in the desulfurization solution, the desulfurized rich desulfurization solution enters a filler oxidation tower, air is blown in at the same time, sodium sulfide in the desulfurization solution reacts with oxygen to generate sodium thiosulfate and sodium sulfate, sodium mercaptan is oxidized to generate sodium hydroxide and disulfide, the sodium hydroxide is dissolved in the desulfurization solution and is circularly used for desulfurization of coal tar, the boiling point of the disulfide is above 109 ℃, the odor threshold value is only below one tenth of that of the mercaptan, when the desulfurization solution is circularly used for desulfurization of the coal tar, the disulfide is dissolved in the coal tar, and hydrogen sulfide, carbonyl sulfide and carbon disulfide in the coal tar are removed, so that the purpose of desulfurization and odor removal of the coal tar is achieved.
The combined process of flash evaporation, nitrogen stripping and mixer pre-alkali washing to remove hydrogen sulfide, liquid membrane contactor to remove carbonyl sulfide, carbon disulfide and low molecular weight mercaptan, dealkalizing coalescence separator to remove free desulfurization liquid and rich desulfurization liquid to catalyze air oxidation regeneration is adopted, hydrogen sulfide in coal tar can be completely removed, the removal rate of carbonyl sulfide and carbon disulfide can reach more than 90%, the removal rate of methyl mercaptan can reach more than 99%, the removal rate of ethyl mercaptan can reach more than 95%, the removal rate of C3 mercaptan can reach more than 80%, the removal rate of C4 mercaptan can reach more than 60%, and the content of free desulfurization liquid carried in refined coal tar does not exceed 10 mug/g. Most of hydrogen sulfide, carbonyl sulfide and carbon disulfide which are volatile and easily cause foul smell in coal tar with the boiling point of below 70 ℃ are removed, and low molecular mercaptan below C4 is converted into disulfide with relatively low odor threshold, so that the purposes of desulfurization and odor removal of the coal tar are achieved, and the emission of desulfurization waste liquid can be greatly reduced.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. The utility model provides a device of coal system tar desulfurization peculiar smell that removes, its characterized in that, includes flash column (1), be equipped with flash column plate (2) in flash column (1), flash column (1) lower part is equipped with flash column gas distributor (3), the coal system tar import on flash column (1) upper portion is connected with coal system tar feed pipe (31), the nitrogen gas import of flash column (1) lower part is connected with nitrogen gas pipe (37), the nitrogen gas import of flash column (1) with flash column gas distributor (3) are connected, the tail gas export at flash column (1) top is connected with flash distillation tail gas pipe (38), the coal system tar export of flash column (1) bottom is connected with coal system tar oil pipe (32) after the flash distillation, the coal-made coke oil pipe (32) after flash evaporation is further connected with a pre-alkali washing mixer (5) and a coal-made tar alkali liquor inlet at the top of the pre-alkali washing tank (6), a coal-made tar outlet at the other side of the top of the pre-alkali washing tank (6) is connected with the coal-made coke oil pipe (33) after hydrogen sulfide removal, an alkali liquor outlet at the bottom of the pre-alkali washing tank (6) is connected with a pre-alkali washing alkali liquor pipe (43), the pre-alkali washing alkali liquor pipe (43) is further connected with a pre-alkali washing pump (7) and the coal-made coke oil pipe (32) after flash evaporation at the inlet of the pre-alkali washing mixer (5), the other end of the coal-made coke oil pipe (33) after hydrogen sulfide removal is connected with a coal-made tar inlet at the top of a primary desulfurization liquid film contactor (8), one-level desulfurization liquid film contactor (8) top side desulfurization liquid inlet connection regeneration desulfurization liquid pipe two (41), one-level desulfurization liquid film contactor (8) is installed on one-level liquid film desulfurization knockout drum (10) through the flange, one-level liquid film desulfurization knockout drum (10) bottom desulfurization liquid exit linkage rich desulfurization liquid pipe (44), one-level liquid film desulfurization knockout drum (10) top opposite side coal system tar exit linkage coal system coking oil pipe (34) after one-level desulfurization, coal system coking oil pipe (34) other end connection second desulfurization liquid film contactor (11) top coal system tar import after one-level desulfurization, second desulfurization liquid film contactor (11) top side desulfurization liquid inlet connection regeneration desulfurization liquid pipe one (40), second desulfurization liquid film contactor (11) is installed on second desulfurization knockout drum (13) through the flange, second liquid film desulfurization knockout drum (13) bottom desulfurization liquid exit linkage rich desulfurization liquid pipe one (45), second desulfurization liquid film knockout drum (13) top opposite side coal system tar exit linkage second desulfurization coal system coking oil pipe (35) after second desulfurization coalescence, second desulfurization liquid film coal system tar oil pipe (35) other end connection tar system coking oil pipe exit (14) refined coal system alkali system coal system liquid outlet (14) bottom (14), rich desulfurization liquid pipe (45) is connected to rich desulfurization liquid pipe two (46) other end, rich desulfurization liquid pipe (44) is connected to rich desulfurization liquid pipe (45) other end, rich desulfurization liquid pipe (44) still is connected with doctor solution heater (16) and doctor solution regenerator tower (17) upper portion doctor solution import, rich desulfurization liquid pipe (44) still is connected with fresh doctor solution pipe (47), fresh doctor solution pipe (47) still is connected with fresh doctor solution tank (23) and fresh doctor solution measuring pump (24), doctor solution regenerator tower (17) lower part air intlet connects compressed air pipe (49), doctor solution regenerator tower (17) upper portion nitrogen intlet connects compressed nitrogen pipe (50), doctor solution regenerator tower (17) top tail gas exit connects doctor solution regeneration tail gas pipe (51), doctor solution regenerator tower (17) bottom doctor solution exit connects regeneration doctor solution pipe (40), regeneration doctor solution pipe (40) still is connected with regeneration doctor solution pipe two (41).
2. The apparatus according to claim 1, wherein a primary liquid membrane contactor core (9) and a secondary liquid membrane contactor core (12) are installed in the primary desulfurization liquid membrane contactor (8) and the secondary desulfurization liquid membrane contactor (11), respectively.
3. The device according to claim 1, characterized in that a coalescing filter element (15) is installed inside the dealkalizing coalescer (14).
4. The device according to claim 1, characterized in that a demister (18) is arranged at the top of the desulfurizing liquid regeneration tower (17), a packing (19) is arranged at the middle section of the desulfurizing liquid regeneration tower (17), and a regeneration tower gas distributor (20) is arranged at the lower part of the desulfurizing liquid regeneration tower (17).
5. The apparatus according to claim 1, characterized in that 10 flash trays (2) are provided in the flash column (1), and the spacing between adjacent flash trays (2) is 400-800mm.
6. The apparatus according to claim 1, wherein the primary desulfurization liquid film contactor (8) and the secondary desulfurization liquid film contactor (11) each comprise a contactor housing (81), a contactor orifice plate (82), a fiber bundle hook (83) and a contactor fiber bundle (84), wherein each contactor fiber bundle (84) corresponds to one fiber bundle hook and one fiber bundle hook hole (85), a plurality of fiber bundle hooks in a straight line are fixed on the contactor orifice plate (82) through one fiber bundle hook cross pin (86), the fiber bundle hook holes (85) on the contactor orifice plate (82) are uniformly distributed, the length of the contactor fiber bundle (84) is 2-10m, the contactor fiber bundle (84) is composed of a large number of fiber filaments with the diameter of 0.2-2.0mm, the surface of the fiber filaments is subjected to chemical modification treatment, the fiber filaments are in a continuous corrugated shape, the height of the corrugations is 2-10mm, and the width of the single-stage corrugations is 5-30mm.
7. The apparatus according to claim 1, wherein the flash column gas distributor (3) and the regeneration column gas distributor (20) are uniformly perforated rows of round or square tubes.
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| CN202221686417.4U CN217757342U (en) | 2022-07-01 | 2022-07-01 | Device for desulfurizing and deodorizing coal tar |
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| CN202221686417.4U CN217757342U (en) | 2022-07-01 | 2022-07-01 | Device for desulfurizing and deodorizing coal tar |
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