CN114939332A - Method and device for removing coke by bubbling and spraying molten salt - Google Patents
Method and device for removing coke by bubbling and spraying molten salt Download PDFInfo
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- 230000005587 bubbling Effects 0.000 title claims abstract description 41
- 238000005507 spraying Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000000571 coke Substances 0.000 title claims abstract description 15
- 238000003860 storage Methods 0.000 claims abstract description 71
- 238000006243 chemical reaction Methods 0.000 claims abstract description 52
- 239000007788 liquid Substances 0.000 claims abstract description 49
- 239000007921 spray Substances 0.000 claims abstract description 32
- 238000012546 transfer Methods 0.000 claims abstract description 11
- 239000006227 byproduct Substances 0.000 claims abstract description 9
- 230000003197 catalytic effect Effects 0.000 claims abstract description 8
- 238000007667 floating Methods 0.000 claims abstract description 7
- 238000004227 thermal cracking Methods 0.000 claims abstract description 4
- 238000005235 decoking Methods 0.000 claims description 48
- 238000010438 heat treatment Methods 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 11
- 239000011229 interlayer Substances 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- 238000005192 partition Methods 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 239000010410 layer Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 229910001369 Brass Inorganic materials 0.000 claims description 3
- 239000010951 brass Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000012265 solid product Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 238000003466 welding Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 3
- 238000002309 gasification Methods 0.000 abstract description 2
- 239000010815 organic waste Substances 0.000 abstract description 2
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- 238000003199 nucleic acid amplification method Methods 0.000 abstract 1
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- 241000197194 Bulla Species 0.000 description 2
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/90—Injecting reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
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- B01D2255/2027—Sodium
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- B01D—SEPARATION
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Abstract
The invention discloses a method and a device for removing coke by bubbling and spraying molten salt, wherein the method for removing coke comprises the steps of carrying out bubbling reaction on tar gas in the molten salt on a bubble cap tower plate through a bubble cap riser of a scale hole bubble cap and a bubble cap scale hole tooth seam after passing through a gas distributor; the tar gas which is not completely reacted and the molten salt sprayed by the spiral spray head are subjected to further heat transfer and catalytic thermal cracking reaction; then the cracked gas escapes from a gas outlet at the top of the bubble-cap reactor and enters a condensing system; the by-product coke in solid state floating on the surface of the molten salt flows into the liquid receiving tray of the next bubble cap tower plate through the overflow weir on the last bubble cap tower plate until the by-product coke flows into the molten salt storage tank. The tar in the cracked gas is eliminated by carrying out multiple countercurrent heat transfer and catalytic cracking on the tar gas passing through the scale hole bubble cap, the molten salt on the bubble cap tower plate and the molten salt sprayed at high temperature, and the like, and the tar removing method is suitable for removing the tar in the organic waste gasification combustible gas and is easy for amplification and industrial production.
Description
Technical Field
The invention relates to the field of energy conversion, in particular to a method and a device for removing coke by bubbling and spraying molten salt.
Background
The warp knitting textile industry is one of the industries which are acknowledged to be seriously polluted, the warp knitting industry in China develops at a high speed, and a large amount of solid wastes in the warp knitting industry cannot be effectively treated. The accumulation of the warp knitting solid wastes in a large quantity not only causes harm to the environment, but also has huge fire-fighting hidden danger, and the direct combustion of the warp knitting solid wastes can generate toxic gas and a large amount of black smoke. The warp knitting solid waste has higher energy, and resources cannot be effectively utilized. The organic matter is pyrolyzed and gasified to be an effective resource utilization method.
Aiming at the main problems of the existing organic matter gasification process, a large amount of liquid by-product tar is generated, the chemical components of the tar are complex, and pipelines and corrosion equipment are easy to block. The conventional methods for treating tar are roughly divided into physical adsorption removal, high-temperature pyrolysis decoking and catalytic decoking. For physical adsorption, the removed tar still generates great harm to the environment and human body without further treatment. For high-temperature pyrolysis, the required temperature is too high, about 1000 ℃, and the requirement on equipment is severe. This patent combines high-temperature pyrolysis and two kinds of methods of catalytic decoking, utilizes high temperature fused salt to carry out catalytic pyrolysis to tar, further strengthens decoking reaction through fused salt spraying and two kinds of ways of tympanic bulla.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an economical, efficient and environment-friendly molten salt bubbling spraying decoking method and device, which can strengthen the mass transfer and heat transfer of tar and molten salt in gas, ensure the efficient and continuous catalytic decoking reaction, improve the production efficiency, are suitable for removing the tar in organic waste gasified combustible gas and are easy to amplify and industrially produce.
The molten salt bubbling spraying decoking method is characterized in that a plurality of horizontally arranged bubble cap tower plates are arranged in a bubble cap reactor for molten salt bubbling spraying decoking, scale hole bubble caps are arranged on the bubble cap tower plates, spiral spray heads and gas distributors are respectively arranged in the top and the bottom of the bubble cap reactor, and the molten salt bubbling spraying decoking method comprises the following steps:
1) heating the molten salt storage tank and the bubble-cap reactor to reach reaction temperature, and introducing N into the bubble-cap reactor through an auxiliary gas inlet pipe and a gas distributor 2 Evacuation of O 2 Starting a molten salt pump to convey the molten salt in the molten salt storage tank to a spiral spray head, spraying the molten salt to a bubble cap tower plate in the bubble cap reactor, adjusting the conveying flow of the molten salt pump to enable gas-liquid two phases to form a stable convection state, and maintaining the temperature of the whole reaction system to be stable;
2) when the reaction temperature is stable, stopping introducing N 2 Starting to introduce tar gas; after passing through the gas distributor, the tar gas is subjected to bubbling reaction in molten salt on a bubble cap tower plate through a bubble cap riser of a scale hole bubble cap and a bubble cap scale hole tooth seam; the incompletely reacted tar gas and the molten salt sprayed by the spiral spray head are subjected to further heat transfer and catalytic thermal cracking reaction; then the cracked gas escapes from a gas outlet at the top of the bubble-cap reactor and enters a condensing system; the byproduct coke in solid state floating on the surface of the fused salt flows into a liquid receiving tray of the next bubble cap tower plate through an overflow weir on the last bubble cap tower plate until the byproduct coke flows into a fused salt storage tank;
3) stopping introducing the tar gas after the reaction is finished, closing the molten salt pump, and introducing N from the auxiliary gas inlet 2 And after the reactor is emptied, the reactor is switched to be filled with air, and carbon deposition in the equipment is removed.
The method for removing the coke by bubbling and spraying the molten salt is characterized in that the molten salt is NaNO 3 、KNO 3 、NaNO 2 、Na 2 CO 3 、K 2 CO 3 、Li 2 CO 3 、Na 2 SO 4 、K 2 SO 4 、Li 2 SO 4 、LiCl、NaCl、KCl、ZnCl 2 Combinations of two or more thereof; the reaction temperature is 220-780 ℃;
KNO is selected as the molten salt 3 And NaNO 3 The reaction temperature is 220-500 ℃ when the mixed molten salt is in a mass ratio of 1: 1.5; na is selected 2 CO 3 、K 2 CO 3 And Li 2 CO 3 The reaction temperature is 380-780 ℃ when the mixed molten salt is in a mass ratio of 1:1: 1.33; selecting KCl and ZnCl 2 The reaction temperature is 285-500 ℃ when the mixed molten salt is in a mass ratio of 1:1.67, and KNO in a mass ratio of 1:1.5 is preferred 3 And NaNO 3 And (4) mixing the molten salt.
The molten salt bubbling spraying decoking method is characterized by further comprising the step of removing carbon deposition in the molten salt storage tank after the reaction in the step 3), wherein the process is as follows: opening a fused salt storage tank opening at the top of the fused salt storage tank, carrying out open heating on the fused salt storage tank, floating the carbon deposit on the surface after fused salt is melted, and then fishing out the carbon deposit.
A fused salt tympanic bulla sprays device that decokes, its characterized in that includes bubble cap reactor, fused salt pump and fused salt storage tank, has the bubble cap column plate that a plurality of levels set up in the bubble cap reactor, is provided with high temperature resistant spiral shower nozzle and gas distributor in the top of bubble cap reactor and the bottom respectively, gas intake pipe penetrates in the bubble cap reactor bottom and is connected with gas distributor, the bubble cap reactor top sets up the pipeline of giving vent to anger and connects condensing system. A plurality of scale hole bubble caps are uniformly distributed on the bubble cap column plate, scale hole tooth gaps are uniformly arranged on the side wall of each scale hole bubble cap along the circumference at intervals, an overflow weir and a downcomer are arranged on one side of each bubble cap column plate, a liquid receiving disc is arranged on the other side of each bubble cap column plate, an inlet is arranged at the upper part of each downcomer, the overflow weir is arranged on the inlet of each downcomer, and the liquid receiving disc of the next bubble cap column plate is arranged right below the downcomer of the previous bubble cap column plate. The outlet of the lower end of the downcomer of the lowermost bubble-cap tower plate is connected with a molten salt storage tank through a side branch pipe, the inlet of a molten salt pump is connected with a liquid inlet pipe, the inlet of the liquid inlet pipe penetrates into the lower end of the molten salt storage tank and keeps a distance of 5-50mm from the bottom wall of the tank, the outlet of the molten salt pump is connected with a liquid outlet pipe, the outlet end of the liquid outlet pipe penetrates into the bubble-cap reactor and is connected with a spiral spray head, and the molten salt pump conveys high-temperature molten salt in the molten salt storage tank to the spiral spray head for spraying.
The device for molten salt bubbling spraying decoking is characterized in that the bubble reactor comprises a reactor inner container, a partition heating jacket is arranged on the outer side of the reactor inner container, a heat-insulating interlayer is arranged on the outer layer of the partition heating jacket, and a reactor shell is arranged on the outer side of the heat-insulating interlayer and used for fixing each part of the reactor; the bubble-cap tower plate and the reactor inner container are both made of high-temperature-resistant nickel alloy and are connected in a welding mode, and the spiral nozzle is made of silicon carbide.
The device for molten salt bubbling spraying decoking is characterized in that the number of bubble cap tower plates in a bubble cap reactor is 1-3, preferably 2-3; the height of an overflow weir on the same bubble cap tower plate is higher than the scale hole tooth gaps of the scale hole bubble caps; the liquid receiving tray and the bubble cap tower plate form an obtuse angle, preferably an included angle of 150 degrees, so that the liquid molten salt flowing onto the liquid receiving tray can flow onto the bubble cap tower plate conveniently.
The overflow weir comprises an overflow weir main body and a fine hole arranged at the lower end of the overflow weir main body; the overflow weir and the bubble cap tower plate are both made of high-temperature-resistant nickel alloy; the number of the holes of the fine holes at the lower end of the overflow weir main body is 2-5, the fine holes are in a shape that two conical cavities are connected, the diameter of the middle hole of each conical cavity is the smallest, the middle hole is gradually expanded towards the left side and the right side in a symmetrical shape, the diameter of the surface hole is the largest, the diameter of the hole of each conical cavity is from 5-15mm of the center diameter to 20-30mm of the surface hole, and molten salt can flow through the holes slowly without being blocked.
The molten salt bubbling spraying decoking device is characterized in that the number of the scale hole bubble covers on the bubble cap tower plate is 3-12, each scale hole bubble cover comprises a gas rising pipe arranged on the bubble cap tower plate and a bubble cap main body arranged on the outer side of the gas rising pipe, scale hole tooth gaps are uniformly arranged on the side wall of the bubble cap main body at intervals along the circumference, the height of the gas rising pipe on the same bubble cap tower plate is higher than the heights of an overflow weir and the scale hole tooth gaps, the scale hole tooth gaps are raised holes which form tooth gap opening directions along the clockwise tangential direction or the counterclockwise tangential direction of the side wall of the bubble cap main body after stamping, tar gas can flow along the clockwise or counterclockwise tangential direction of the side wall of the bubble cap main body through the gas rising pipes through the scale hole tooth gaps, so that the molten salt forms local countercurrent around the bubble cap main body, and the gas-liquid contact effect is strengthened.
The device for molten salt bubbling spraying decoking is characterized in that the riser is connected with the bubble cap main body through a support piece, one end of the support piece is fixedly arranged on the riser, and the other end of the support piece is fixedly installed on the top of the bubble cap main body through a fixing bolt, so that the bubble cap main body is suspended on the outer side of the riser, wherein the lower end of the bubble cap main body is provided with an opening; the top of the bubble cap main body is also connected with a liquid shielding cover through a support rod, the support rod is strip-shaped high-temperature-resistant nickel alloy, the lower end of the support rod is welded with the bubble cap shell main body, and the upper end of the support rod is detachably connected with the liquid shielding cover, so that the molten salt liquid is prevented from contacting a fixing bolt; the liquid shielding cover is made of umbrella-shaped high-temperature-resistant nickel alloy.
The device for molten salt bubbling spray decoking is characterized by further comprising a temperature sensor, wherein the temperature sensor is connected with a first thermocouple, a second thermocouple and a third thermocouple, the temperature measuring end of the first thermocouple extends into the upper part of the bubble-cap reactor, and the temperature measuring end of the third thermocouple extends into the outlet at the lower end of a downcomer of the lowermost bubble-cap tower plate and is used for measuring the temperature of molten salt flowing to a molten salt storage tank; the temperature measuring end of the second thermocouple extends into the lower end of the molten salt storage tank and is used for measuring the temperature of the molten salt in the storage tank.
The molten salt storage tank is provided with a molten salt storage tank opening and an emptying pipeline, the molten salt storage tank opening is positioned above the molten salt storage tank and consists of a detachable sealing cover and a tank body, and the emptying pipeline is positioned below the molten salt storage tank and consists of a high-temperature-resistant pipeline and a brass valve; the molten salt storage tank has the function of heating and heat preservation.
The device for molten salt bubbling spraying decoking is characterized in that the side part of a gas inlet pipe is connected with an auxiliary inlet pipe, a return gas pipeline is arranged between a gas outlet pipeline and the gas inlet pipe, and a high-temperature gas pipeline pump is arranged at one end, close to the gas outlet pipeline, of the return gas pipeline and used for returning a part of discharged pyrolysis gas back to a bubble reactor through the return gas pipeline.
By adopting the technology, compared with the prior decoking technology, the decoking technology has the following gain effects:
1) according to the invention, through the multi-layer tower plate and the plurality of scale hole tooth seam bubble caps, tar in gas repeatedly exchanges heat with high-temperature molten salt bubbling through the scale hole tooth seams of the multi-layer tower plate, tar gas is converted into solid coke and noncondensable gas as much as possible, tar components in the gas are greatly reduced or even completely eliminated, and meanwhile, the gas flowing out through the scale hole tooth seams can generate a disturbance effect on the molten salt around the bubble caps to generate local countercurrent. On one hand, the contact between the gas and the molten salt can be strengthened, the catalytic function of the molten salt can be exerted to the greatest extent, and the temperature is greatly reduced compared with the traditional decoking reaction; on the other hand, the solid product around the bubble cap can be blown away, and the normal operation of the decoking reaction is ensured. Compared with the daily average treatment capacity of the traditional similar reactor, the device has greatly improved operation flexibility.
2) The spraying device is additionally arranged above the reactor, so that the mass transfer and heat transfer of the gas and the molten salt are enhanced again, the sprayed molten salt and the tar gas which is not completely reacted in the gas are subjected to multidimensional mass transfer and heat transfer, and the tar in the gas is completely removed as far as possible. And thirdly, the sprayed molten salt is gathered on the tower plate, coke floating on the surface of the molten salt is brought to the next tower plate through an overflow weir until the coke is sent to a molten salt storage tank and is gathered on the surface layer of the molten salt in the molten salt storage tank, and the coke on the surface layer is subsequently and intensively removed. Compared with the traditional similar device, the device provided by the invention has the advantages that the fused salt is circulated and refluxed in the reactor, the fused salt of the device provided by the invention adopts an overflow separation and refluxing flow, the decoking reaction is ensured to be continuously and stably carried out, and the tar content in the gas at the gas outlet is obviously reduced.
3) The invention can make the fused salt flow through the pores slowly by drilling a plurality of pores at the bottom of the bubble cap tower plate overflow weir, stop spraying after the reaction is finished, and make the fused salt liquid gathered on the tower plate flow into the bottom tower plate through the pores at the bottom of the overflow weir until the fused salt liquid completely flows to the fused salt storage tank.
4) According to the invention, the umbrella-shaped flow shielding cover is additionally arranged above the scale hole bubble cover, so that the direct contact between the easily damaged structures such as bolts and nuts above the bubble cover and high-temperature molten salt can be avoided, the loss of easily damaged parts is reduced, and the service life of the reactor is greatly prolonged compared with that of the traditional reactor bubble cover.
Drawings
FIG. 1 is a schematic flow diagram of a molten salt bubbling spray decoking method constructed by the invention
FIG. 2 is a schematic structural diagram of a molten salt bubbling spray decoking reaction device constructed according to the invention;
FIG. 3 is a schematic structural diagram of a scale hole bubble cap in a molten salt bubbling spray decoking reaction device constructed according to the invention;
FIG. 4 is a schematic structural diagram of a bubble cap tray in a molten salt bubbling spray decoking reaction device constructed according to the present invention;
FIG. 5 is a schematic structural diagram of a fine-meshed overflow weir in a molten salt bubbling spray decoking reaction device constructed according to the invention;
reference numerals: 1-reactor inner container, 2-bubble cap tray, 202-downcomer, 203-overflow weir, 2031-overflow weir main body, 2032-pore, 204-liquid receiving disc, 3-scale hole bubble cap, 301-riser, 302-scale hole tooth seam, 303-bubble cap main body, 304-supporting rod, 305-liquid shielding cover, 4-clapboard heating jacket, 5-fused salt storage tank, 502-fused salt storage tank opening, 6-fused salt pump, 7-spiral spray head, 8-temperature sensor, 801-first thermocouple, 802-second thermocouple, 803-third thermocouple, 9-gas inlet pipe, 901-gas distributor, 10-gas outlet pipe, 11-reflux gas pipe, 12-high temperature gas pipe pump, 13-heat preservation interlayer, 14-reactor shell, 15-auxiliary inlet pipe.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1:
referring to fig. 1, a molten salt bubbling spray decoking method comprises a process of reacting tar gas with molten salt bubbling through a scale-hole bubble cap; reacting the tar gas with the molten salt sprayed by the spiral spray head; the process that the fused salt carries the carbon deposit to flow back to the fused salt storage tank; the molten salt regeneration process is carried out by heating the opening of the molten salt storage tank; the method comprises the following specific steps:
1) heating the molten salt storage tank 5 and the bubble-cap reactor to reach the reaction temperature, and introducing N into the bubble-cap reactor through an auxiliary gas inlet pipe 15 by a gas distributor 901 2 Evacuation of O 2 Starting a molten salt pump 6 to convey the molten salt in a molten salt storage tank 5 to a spiral nozzle 7, spraying the molten salt to a bubble cap tower plate 2 in the bubble cap reactor, adjusting the conveying flow of the molten salt pump 6 to enable gas-liquid two phases to form a stable convection state, and maintaining the whole reactionThe temperature of the reaction system is stable;
2) stopping introducing N when the reaction temperature is stable 2 Starting to introduce tar gas; after passing through the gas distributor, the tar gas is subjected to bubbling reaction in molten salt on the bubble-cap tower plate 2 through a bubble-cap gas riser 301 and a bubble-cap scale-hole tooth seam 302 of the scale-hole bubble cap 3; the incompletely reacted tar gas and the molten salt sprayed by the spiral spray nozzle 7 are subjected to further heat transfer and catalytic thermal cracking reaction; then the cracked gas escapes from a gas outlet at the top of the bubble-cap reactor and enters a condensing system; the byproduct, namely solid product coke, floats on the surface of the molten salt and flows into a liquid receiving disc of a next bubble cap tower plate through an overflow weir on the last bubble cap tower plate until the byproduct flows into a molten salt storage tank 5;
3) stopping introducing the tar gas after the reaction is finished, closing the molten salt pump 6, and introducing N from the auxiliary gas inlet 15 2 And after the reactor is emptied, the reactor is switched to be filled with air, and carbon deposition in the equipment is removed. And then closing the auxiliary air inlet pipeline 15, opening a molten salt storage tank opening 502 at the top of the molten salt storage tank 5, carrying out open heating on the molten salt storage tank 5, floating carbon deposits on the surface after molten salt is melted, and fishing out the carbon deposits. And after the reaction is finished, all power supplies are turned off, and the reaction is finished.
The molten salt is NaNO 3 、KNO 3 、NaNO 2 、Na 2 CO 3 、K 2 CO 3 、Li 2 CO 3 、Na 2 SO 4 、K 2 SO 4 、Li 2 SO 4 、LiCl、NaCl、KCl、ZnCl 2 Combinations of two or more thereof; the reaction temperature is 220-780 ℃; KNO is selected as the molten salt 3 And NaNO 3 The reaction temperature is 220-500 ℃ when the mixed molten salt is in a mass ratio of 1: 1.5; selecting Na 2 CO 3 、K 2 CO 3 And Li 2 CO 3 The reaction temperature is 380-780 ℃ when the mixed molten salt is in a mass ratio of 1:1: 1.33; selecting KCl and ZnCl 2 The reaction temperature is 285-500 ℃ when the mixed molten salt is in a mass ratio of 1:1.67, and KNO in a mass ratio of 1:1.5 is preferred 3 And NaNO 3 And (4) mixing the molten salt.
Referring to fig. 2, the bubble reactor comprises a reactor inner container 1, a partition heating jacket 4 outside the reactor inner container 1, a heat insulating interlayer 13 arranged on the outer layer of the partition heating jacket 4, and a reactor shell 14 arranged outside the heat insulating interlayer 13 for fixing each part of the reactor.
The device comprises a bubble-cap reactor, a molten salt pump 6, a molten salt storage tank 5 and a temperature sensor 8 for monitoring the temperature of the whole equipment, wherein a plurality of horizontally arranged bubble-cap tower plates 2 are arranged in the bubble-cap reactor, a high-temperature resistant spiral spray head 7 and a gas distributor 901 are respectively arranged in the top and the bottom of the bubble-cap reactor, a gas inlet pipe 9 penetrates into the bottom of the bubble-cap reactor and is connected with the gas distributor 901, and an air outlet pipeline 10 is arranged at the top of the bubble-cap reactor and is connected with a condensing system. A plurality of scale hole bubble caps 3 are uniformly distributed on the bubble cap tower plate 2, scale hole tooth gaps 302 are uniformly arranged on the side wall of each scale hole bubble cap 3 along the circumference at intervals, an overflow weir 203 and a downcomer 202 are arranged on one side of the bubble cap tower plate 2, a liquid receiving disc 204 is arranged on the other side of the bubble cap tower plate, an inlet is arranged at the upper part of the downcomer, the overflow weir is arranged on the inlet of the downcomer, and the liquid receiving disc of the next bubble cap tower plate is arranged right below the downcomer of the previous bubble cap tower plate. The outlet of the lower end of the downcomer of the lowermost bubble cap tower plate is connected with the molten salt storage tank 5 through a side branch pipe 501, the inlet of a molten salt pump 6 is connected with a liquid inlet pipe 601, the inlet of the liquid inlet pipe 601 penetrates into the lower end of the molten salt storage tank 5 and keeps a distance of 5-50mm with the bottom wall of the tank, the outlet of the molten salt pump 6 is connected with a liquid outlet pipe 602, the outlet end of the liquid outlet pipe 602 penetrates into the bubble cap reactor and is connected with a spiral spray nozzle 7, and the molten salt pump 6 conveys high-temperature molten salt in the molten salt storage tank (5) to the spiral spray nozzle 7 for spraying.
The number of bubble cap trays 2 in the bubble cap reactor is 1 to 3, preferably 2 to 3; the overflow weir 203 on the same bubble cap tray 2 is higher than the scale hole tooth gaps 302 of the scale hole bubble caps 3; an obtuse angle, preferably 150 degrees, is formed between the liquid receiving tray 204 and the bubble cap tray 2, so that the liquid molten salt flowing onto the liquid receiving tray 204 can flow onto the bubble cap tray 2 conveniently.
The overflow weir 203 includes an overflow weir main body 2031 and a fine hole 2032 provided at a lower end of the overflow weir main body 2031; the overflow weir 203 and the bubble cap tower plate are both made of high-temperature-resistant nickel alloy; the number of the holes of the fine holes 2032 at the lower end of the overflow weir main body 2031 is 2-5, the fine holes 2032 are in a shape that two conical cavities are connected, the diameter of the middle hole of each conical cavity is the smallest, the middle hole is gradually enlarged towards the left side and the right side in a symmetrical shape, the diameter of the surface hole is the largest, the diameter of the hole of each conical cavity is from 5-15mm at the center to 20-30mm at the surface, and molten salt can flow through slowly without being blocked.
The number of the scale hole bubble caps 3 on the bubble cap tray 2 is 3-12, each scale hole bubble cap 3 comprises an air lifting pipe 301 arranged on the bubble cap tray 2 and a bubble cap main body 303 arranged on the air lifting pipe 301, scale hole tooth gaps 302 are uniformly arranged on the side wall of each bubble cap main body 303 along the circumference at intervals, the height of the air lifting pipe 301 on the same bubble cap tray 2 is higher than that of the overflow weir 203 and the scale hole tooth gaps 302, the scale hole tooth gaps 302 are raised holes which form the tooth gap opening direction along the clockwise tangential direction or the anticlockwise tangential direction of the side wall of the bubble cap main body 303 after stamping, tar gas can flow from the air lifting pipe 301 along the clockwise or anticlockwise tangential direction of the side wall of the bubble cap main body 303 through the scale hole tooth gaps 302, so that molten salt forms local countercurrent around the bubble cap main body 303, and the gas-liquid contact effect is enhanced.
The gas rising pipe 301 is connected with the blister main body 303 through a supporting piece, one end of the supporting piece is fixedly arranged on the gas rising pipe 301, and the other end of the supporting piece is fixedly installed on the top of the blister main body 303 through a fixing bolt 306; the top of the bubble cap main body 303 is also connected with a liquid shielding cover 305 through a support rod 304, the support rod 304 is strip-shaped high-temperature-resistant nickel alloy, the lower end of the support rod 304 is welded with the bubble cap shell main body, and the upper end of the support rod is detachably connected with the liquid shielding cover 305, so that the molten salt liquid is prevented from contacting with a fixing bolt 306; the liquid-shielding cover 305 is an umbrella-shaped high-temperature-resistant nickel alloy.
The temperature sensor 8 is connected with a first thermocouple 801, a second thermocouple 802 and a third thermocouple 803, the temperature measuring end of the first thermocouple 801 extends into the upper part of the bubble cap reactor, and the temperature measuring end of the third thermocouple 803 extends into the outlet of the lower end of the downcomer of the lowermost bubble cap tray to measure the temperature of the molten salt flowing to the molten salt storage tank 5; the temperature measuring end of the second thermocouple 802 extends into the lower end of the molten salt storage tank 5 and is used for measuring the temperature of the molten salt in the storage tank.
The molten salt storage tank 5 is provided with a molten salt storage tank opening 502 and a venting pipeline 503, the molten salt storage tank opening 502 is positioned above the molten salt storage tank and consists of a detachable sealing cover and a tank body, and the venting pipeline 503 is positioned below the molten salt storage tank and consists of a high-temperature-resistant pipeline and a brass valve; the molten salt storage tank 5 has the function of heating and heat preservation.
The side of the gas inlet pipe 9 is connected with an auxiliary gas inlet pipe 15, a return gas pipeline 11 is arranged between the gas outlet pipeline 10 and the gas inlet pipe 9, and a high-temperature gas pipeline pump 12 is arranged at one end of the return gas pipeline 11 close to the gas outlet pipeline 10, and is used for returning a part of the discharged pyrolysis gas back to the bubble reactor through the return gas pipeline 11.
Example 2: molten salt bubbling spray decoking
The decoking reaction was carried out by using the method of the flow shown in FIG. 1 and the apparatus of the structure shown in FIG. 2, by first heating a molten salt storage tank containing 2kg of nitrate, KNO 3 ，NaNO 3 The mass ratio of (A) to (B) is 1: 1.5. When the temperature of the storage tank is heated to 450 ℃, N with the speed of 0.5L/min begins to be introduced into the reactor 2 And starting the reactor to heat. When the temperature of 3 thermocouples is stable to 450 ℃, the molten salt pump is started after the temperature is kept constant for 30 minutes, the molten salt is sprayed into the reactor, the flow of the molten salt pump is adjusted, the flow of the molten salt flowing into and out of the molten salt storage tank is stable, and the N is stopped from being introduced 2 And (3) introducing tar gas, reacting, wherein one part of the gas outlet flows back to the gas inlet, and the other part of the gas outlet enters a subsequent condensing system.
Example 3: cleaning and maintenance of decoking apparatus
Example 2 continuous decoking reaction about 20 days, the detection results show that the efficiency of the decoking reactor is reduced, the tar gas generating device is stopped, the return pipeline pump and the molten salt pump are closed, and N is introduced at 1.2L/min 2 After 10min, air is introduced at a rate of 1.2L/min to heat for 2h after other gases in the reactor are exhausted, and when CO and CO in the cracked gas 2 The content is below 5 percent, then the aeration is stopped, the opening of the molten salt storage tank is opened, the carbon deposit floating on the surface of the molten salt is manually skimmed, and then the decoking reaction in the example 2 is continued, and the result shows that the decoking efficiency is close to that of the example 2.
In the prior art, the tar gas is directly blown into the molten salt, the conversion rate of the tar gas basically reaches 90%, but the conversion rate of the tar gas adopting the method of the embodiment 2 of the invention can be further improved by more than 5%, and the stability of decoking operation is greatly improved.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (10)
1. The molten salt bubbling spraying decoking method is characterized in that a plurality of horizontally arranged bubble-cap tower plates (2) are arranged in a bubble-cap reactor for molten salt bubbling spraying decoking, scale-hole bubble caps (3) are arranged on the bubble-cap tower plates (2), a spiral spray head (7) and a gas distributor (901) are respectively arranged in the top and the bottom of the bubble-cap reactor, and the molten salt bubbling spraying decoking method comprises the following steps:
1) heating the molten salt storage tank (5) and the bubble-cap reactor to reach reaction temperature, and introducing N into the bubble-cap reactor through an auxiliary gas inlet pipe (15) through a gas distributor (901) 2 Evacuation of O 2 Starting a molten salt pump (6) to convey the molten salt in the molten salt storage tank (5) to a spiral spray nozzle (7), spraying the molten salt to a bubble cap tower plate (2) in the bubble cap reactor, adjusting the conveying flow of the molten salt pump (6) to enable gas-liquid two phases to form a stable convection state, and maintaining the temperature of the whole reaction system to be stable;
2) stopping introducing N when the reaction temperature is stable 2 Starting to introduce tar gas; after passing through a gas distributor, the tar gas is subjected to bubbling reaction in molten salt on a bubble cap tower plate (2) through a bubble cap riser (301) of a scale hole bubble cap (3) and a bubble cap scale hole tooth seam (302); the incompletely reacted tar gas and the molten salt sprayed by the spiral spray nozzle (7) are subjected to further heat transfer and catalytic thermal cracking reaction; then the cracked gas escapes from a gas outlet at the top of the bubble-cap reactor and enters a condensing system; the byproduct, namely solid product coke, floats on the surface of the molten salt and flows into a liquid receiving disc of a next bubble cap tower plate through an overflow weir on the last bubble cap tower plate until the byproduct flows into a molten salt storage tank (5);
3) stopping introducing the tar gas after the reaction is finished, closing the molten salt pump (6), and introducing N from the auxiliary gas inlet (15) 2 After the reactor is emptied, the reactor is switched to be introducedAir, and carbon deposit in the equipment is removed.
2. The molten salt bubbling spray decoking method according to claim 1, wherein the molten salt is NaNO 3 、KNO 3 、NaNO 2 、Na 2 CO 3 、K 2 CO 3 、Li 2 CO 3 、Na 2 SO 4 、K 2 SO 4 、Li 2 SO 4 、LiCl、NaCl、KCl、ZnCl 2 Combinations of two or more thereof; the reaction temperature is 220-780 ℃;
KNO is selected as the molten salt 3 And NaNO 3 The reaction temperature is 220-500 ℃ when the mixed molten salt is in a mass ratio of 1: 1.5; na is selected 2 CO 3 、K 2 CO 3 And Li 2 CO 3 The reaction temperature is 380-780 ℃ when the mixed molten salt is in a mass ratio of 1:1: 1.33; selecting KCl and ZnCl 2 The reaction temperature is 285-500 ℃ when the mixed molten salt is in a mass ratio of 1:1.67, and KNO in a mass ratio of 1:1.5 is preferred 3 And NaNO 3 Mixing the molten salt.
3. The molten salt bubbling spraying decoking method as claimed in claim 1, characterized by further comprising a step of removing carbon deposits in the molten salt storage tank (5) after the reaction in step 3) is finished, and the process is as follows: opening a fused salt storage tank opening (502) at the top of the fused salt storage tank (5), carrying out open heating on the fused salt storage tank (5), floating the carbon deposit on the surface after the fused salt is melted, and then fishing out the carbon deposit.
4. The device for molten salt bubbling spraying decoking is characterized by comprising a bubble reactor, a molten salt pump (6) and a molten salt storage tank (5), wherein a plurality of bubble tower plates (2) which are horizontally arranged are arranged in the bubble reactor, a high-temperature-resistant spiral spray head (7) and a gas distributor (901) are respectively arranged in the top and the bottom of the bubble reactor, a gas inlet pipe (9) penetrates into the bottom of the bubble reactor and is connected with the gas distributor (901), and a gas outlet pipeline (10) is arranged at the top of the bubble reactor and is connected with a condensing system;
a plurality of scale hole bubble caps (3) are uniformly distributed on the bubble cap tower plate (2), scale hole tooth gaps (302) are uniformly arranged on the side wall of each scale hole bubble cap (3) at intervals along the circumference, an overflow weir (203) and a downcomer (202) are arranged on one side of the bubble cap tower plate (2), a liquid receiving disc (204) is arranged on the other side of the bubble cap tower plate, an inlet is arranged at the upper part of the downcomer, the overflow weir is arranged on the inlet of the downcomer, and the liquid receiving discs of the next bubble cap tower plate correspond to the position under the downcomer of the previous bubble cap tower plate;
the downcomer lower extreme export of below bubble cap column plate is connected with fused salt storage tank (5) through lateral part branch pipe (501), fused salt pump (6) access connection feed liquor pipe (601), inside feed liquor pipe (601) entry penetrated to fused salt storage tank (5) lower extreme, and keep 5-50 mm's distance with the tank bottoms wall, fused salt pump (6) exit linkage drain pipe (602), drain pipe (602) exit end penetrates to bubble cap reactor inside and is connected with spiral spray nozzle (7), fused salt pump (6) carry the high temperature fused salt in fused salt storage tank (5) to spiral spray nozzle (7).
5. The molten salt bubbling spraying decoking device according to claim 4, characterized in that the bubble reactor comprises a reactor inner container (1), a partition heating jacket (4) outside the reactor inner container (1), a heat-insulating interlayer (13) is arranged on the outer layer of the partition heating jacket (4), and a reactor outer shell (14) is arranged outside the heat-insulating interlayer (13) for fixing each component of the reactor; the bubble cap tower plate (2) and the reactor inner container (1) are both made of high-temperature-resistant nickel alloy and are connected in a welding mode, and the spiral nozzle (7) is made of silicon carbide.
6. A molten salt bubbling sparger decoking apparatus as claimed in claim 4, in which the number of bubble cap trays (2) in the bubble cap reactor is from 1 to 3, preferably from 2 to 3; the height of an overflow weir (203) on the same bubble cap tray (2) is higher than the height of a scale hole tooth gap (302) of the scale hole bubble cap (3); an obtuse angle, preferably an included angle of 150 degrees, is formed between the liquid receiving disc (204) and the bubble cap tower plate (2), so that the liquid molten salt flowing onto the liquid receiving disc (204) can flow onto the bubble cap tower plate (2) conveniently;
the overflow weir (203) comprises an overflow weir main body (2031) and a pore (2032) arranged at the lower end of the overflow weir main body (2031); the overflow weir (203) and the bubble cap tower plate are both made of high-temperature-resistant nickel alloy; the number of the holes of the fine holes (2032) at the lower end of the overflow weir main body (2031) is 2-5, the fine holes (2032) are in a shape that two conical cavities are connected, the diameter of the middle opening of each conical cavity is the smallest, the middle opening is gradually enlarged towards the left side and the right side in a symmetrical shape, the diameter of the surface opening is the largest, and the diameter of the opening of each conical cavity is from 5-15mm to 20-30mm, so that molten salt can flow through slowly without being blocked.
7. The molten salt bubbling spray decoking device as claimed in claim 4, wherein the number of the scale-hole bubble caps (3) on the bubble cap tray (2) is 3-12, the scale-hole bubble caps (3) comprise a gas riser (301) arranged on the bubble cap tray (2) and a bubble cap main body (303) arranged outside the gas riser (301), scale-hole tooth gaps (302) are uniformly arranged on the side wall of the bubble cap main body (303) along the circumference at intervals, the height of the gas riser (301) on the same bubble cap tray (2) is higher than the height of the overflow weir (203) and the scale-hole tooth gaps (302), the scale-hole tooth gaps (302) are convex holes which are punched to form a tooth gap opening direction along the clockwise tangential direction or the counterclockwise tangential direction of the side wall of the bubble cap main body (303), so that tar gas can flow from the gas riser (301) through the scale-hole tooth gaps (302) along the clockwise or counterclockwise tangential direction of the side wall of the bubble cap main body (303), so that the molten salt forms local countercurrent around the bubble cap main body (303) to enhance the gas-liquid contact effect.
8. The molten salt bubbling spray decoking device as claimed in claim 7, wherein the gas lift pipe (301) is connected with the bubble cap main body (303) through a support, one end of the support is fixedly arranged on the gas lift pipe (301), and the other end of the support is fixedly installed on the top of the bubble cap main body (303) through a fixing bolt (306), so that the bubble cap main body (303) is suspended outside the gas lift pipe (301), wherein the lower end of the bubble cap main body (303) is open; the top of the bubble cap main body (303) is also connected with a liquid shielding cover (305) through a support rod (304), the support rod (304) is strip-shaped high-temperature-resistant nickel alloy, the lower end of the support rod is welded with the bubble cap shell main body, and the upper end of the support rod is detachably connected with the liquid shielding cover (305), so that the molten salt liquid is prevented from contacting with a fixing bolt (306); the liquid shielding cover (305) is an umbrella-shaped high-temperature-resistant nickel alloy.
9. The molten salt bubbling spray decoking device according to claim 4, characterized by further comprising a temperature sensor (8), wherein the temperature sensor (8) is connected with a first thermocouple (801), a second thermocouple (802) and a third thermocouple (803), the temperature measuring end of the first thermocouple (801) extends into the upper part of the bubble-cap reactor, and the temperature measuring end of the third thermocouple (803) extends into the outlet at the lower end of the downcomer of the lowermost bubble-cap tray for measuring the temperature of the molten salt flowing to the molten salt storage tank (5); the temperature measuring end of the second thermocouple (802) extends into the lower end of the molten salt storage tank (5) and is used for measuring the temperature of the molten salt in the storage tank;
the molten salt storage tank (5) is provided with a molten salt storage tank opening (502) and an emptying pipeline (503), the molten salt storage tank opening (502) is positioned above the molten salt storage tank and consists of a detachable sealing cover and a tank body, and the emptying pipeline (503) is positioned below the molten salt storage tank and consists of a high-temperature-resistant pipeline and a brass valve; the molten salt storage tank (5) has the functions of heating and heat preservation.
10. The molten salt bubbling spraying decoking device according to claim 4, characterized in that an auxiliary gas inlet pipe (15) is connected to the side of the gas inlet pipe (9), a return gas pipe (11) is arranged between the gas outlet pipe (10) and the gas inlet pipe (9), and a high-temperature gas pipe pump (12) is arranged at one end of the return gas pipe (11) close to the gas outlet pipe (10) and used for returning a part of the discharged pyrolysis gas back flow into the bubble reactor again through the return gas pipe (11).
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| CN202210673756.7A CN114939332A (en) | 2022-06-15 | 2022-06-15 | Method and device for removing coke by bubbling and spraying molten salt |
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